# SUBMISSION DETAILS _publ_contact_author_name 'Hern\'andez-Ortega Simon' _publ_contact_author_address ; Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Cd. Universitaria, Circuito Exterior, Coyoac\'an, C.P. 04510, M\'exico D.F., M\'exico ; _publ_contact_author_email simonho@unam.mx _publ_contact_author_fax '+525556162203' _publ_contact_author_phone '+525556224515' _publ_contact_letter ; ? ; _publ_requested_journal organometallics _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Coordination of 12 electrons organometallic fragments to the arene ring of non-symmetric group 10 POCOP pincer complexes. . ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # NB if using publCIF, the Author database tool might prove useful # (see the Tools menu in publCIF) loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Espinosa-Jalapa, Noel Ángel ' . ; Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Cd. Universitaria, Circuito Exterior, Coyoac\'an, C.P. 04510, M\'exico D.F., M\'exico ; 'Hern\'andez-Ortega Simon' . ; Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Cd. Universitaria, Circuito Exterior, Coyoac\'an, C.P. 04510, M\'exico D.F., M\'exico ; 'Le Goff, Xavier F.' . ; Laboratoire Heteroelements et Coordination, Ecole Polytechnique, CNRS F-91128 Palaiseau Cedex France ; 'Djukic, Jean-Pierre' . ; Institut de Chimie de Strasbourg, UMR CNRS 7177, Université de Strasbourg, 4 rue Blaise Pascal, 67000 Strasbourg, France ; 'Morales-Morales David' . ; Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Cd. Universitaria, Circuito Exterior, Coyoac\'an, C.P. 04510, M\'exico D.F., M\'exico ; 'Le Lagadec, Ronan' . ; Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Cd. Universitaria, Circuito Exterior, Coyoac\'an, C.P. 04510, M\'exico D.F., M\'exico ; #============================================================================== data_compound-2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H33 Cl Ni O2 P2' _chemical_formula_sum 'C22 H33 Cl Ni O2 P2' _chemical_formula_weight 485.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.573(2) _cell_length_b 8.5014(8) _cell_length_c 25.957(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.8970(10) _cell_angle_gamma 90.00 _cell_volume 4977.2(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.35 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.6785 _exptl_absorpt_correction_T_max 0.8017 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector 01-670' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 39672 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.37 _reflns_number_total 9108 _reflns_number_gt 7286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _solved_by 'Simon Hernandez-Ortega' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9108 _refine_ls_number_parameters 564 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.652127(11) 0.34669(3) 0.012068(10) 0.03988(9) Uani 1 1 d . . . Cl1 Cl 0.59587(3) 0.51779(8) -0.04223(3) 0.0723(2) Uani 1 1 d . . . P1 P 0.62319(2) 0.38853(6) 0.08246(2) 0.04097(14) Uani 1 1 d . . . P2 P 0.68855(3) 0.23944(7) -0.04614(2) 0.04559(14) Uani 1 1 d . B . O1 O 0.66674(6) 0.27958(17) 0.13077(5) 0.0459(3) Uani 1 1 d . . . O2 O 0.74457(7) 0.13027(18) -0.01196(6) 0.0547(4) Uani 1 1 d . . . C1 C 0.70577(9) 0.1897(2) 0.11167(8) 0.0397(5) Uani 1 1 d . . . C2 C 0.70456(8) 0.2076(2) 0.05865(8) 0.0378(4) Uani 1 1 d . . . C3 C 0.74595(9) 0.1160(2) 0.04191(8) 0.0432(5) Uani 1 1 d . . . C4 C 0.78570(9) 0.0178(3) 0.07463(9) 0.0501(5) Uani 1 1 d . . . H4 H 0.8126 -0.0379 0.0616 0.060 Uiso 1 1 calc R . . C5 C 0.82536(10) -0.1005(3) 0.16513(10) 0.0568(6) Uani 1 1 d . . . H5 H 0.8537 -0.1550 0.1536 0.068 Uiso 1 1 calc R . . C6 C 0.82307(11) -0.1202(3) 0.21610(11) 0.0634(7) Uani 1 1 d . . . H6 H 0.8493 -0.1892 0.2390 0.076 Uiso 1 1 calc R . . C7 C 0.78168(11) -0.0380(3) 0.23470(9) 0.0614(6) Uani 1 1 d . . . H7 H 0.7802 -0.0530 0.2698 0.074 Uiso 1 1 calc R . . C8 C 0.74347(10) 0.0642(3) 0.20160(9) 0.0519(6) Uani 1 1 d . . . H8 H 0.7164 0.1197 0.2145 0.062 Uiso 1 1 calc R . . C9 C 0.74440(9) 0.0869(2) 0.14816(8) 0.0410(5) Uani 1 1 d . . . C10 C 0.78566(9) 0.0012(2) 0.12887(9) 0.0437(5) Uani 1 1 d . . . C11 C 0.54967(10) 0.3153(3) 0.07923(9) 0.0535(6) Uani 1 1 d . . . H11 H 0.5209 0.3877 0.0562 0.064 Uiso 1 1 calc R . . C12 C 0.54038(14) 0.1555(4) 0.05157(14) 0.0902(10) Uani 1 1 d . . . H12A H 0.5700 0.0834 0.0715 0.135 Uiso 1 1 calc R . . H12B H 0.5435 0.1661 0.0157 0.135 Uiso 1 1 calc R . . H12C H 0.5017 0.1163 0.0501 0.135 Uiso 1 1 calc R . . C13 C 0.53724(12) 0.3116(4) 0.13331(11) 0.0814(9) Uani 1 1 d . . . H13A H 0.4971 0.2781 0.1285 0.122 Uiso 1 1 calc R . . H13B H 0.5427 0.4150 0.1489 0.122 Uiso 1 1 calc R . . H13C H 0.5640 0.2395 0.1568 0.122 Uiso 1 1 calc R . . C14 C 0.63122(11) 0.5804(3) 0.11500(10) 0.0587(6) Uani 1 1 d . . . H14 H 0.6284 0.5654 0.1516 0.070 Uiso 1 1 calc R . . C15 C 0.69244(15) 0.6452(4) 0.11931(14) 0.0952(10) Uani 1 1 d . . . H15A H 0.6958 0.6644 0.0839 0.143 Uiso 1 1 calc R . . H15B H 0.7220 0.5703 0.1375 0.143 Uiso 1 1 calc R . . H15C H 0.6982 0.7419 0.1393 0.143 Uiso 1 1 calc R . . C16 C 0.58194(15) 0.6925(3) 0.08595(13) 0.0969(11) Uani 1 1 d . . . H16A H 0.5886 0.7937 0.1031 0.145 Uiso 1 1 calc R . . H16B H 0.5445 0.6517 0.0874 0.145 Uiso 1 1 calc R . . H16C H 0.5817 0.7027 0.0491 0.145 Uiso 1 1 calc R . . C17 C 0.64084(12) 0.0969(3) -0.09076(10) 0.0720(7) Uani 1 1 d DU . . H17 H 0.6624 0.0532 -0.1145 0.086 Uiso 1 1 calc R A 1 C18 C 0.5826(4) 0.1673(15) -0.1258(5) 0.116(3) Uani 0.72(3) 1 d PDU B 1 H18A H 0.5910 0.2550 -0.1457 0.174 Uiso 0.72(3) 1 calc PR B 1 H18B H 0.5592 0.2022 -0.1032 0.174 Uiso 0.72(3) 1 calc PR B 1 H18C H 0.5610 0.0889 -0.1504 0.174 Uiso 0.72(3) 1 calc PR B 1 C19 C 0.6290(6) -0.0377(10) -0.0550(4) 0.094(2) Uani 0.72(3) 1 d PDU B 1 H19A H 0.6661 -0.0811 -0.0338 0.141 Uiso 0.72(3) 1 calc PR B 1 H19B H 0.6060 -0.1185 -0.0774 0.141 Uiso 0.72(3) 1 calc PR B 1 H19C H 0.6077 0.0029 -0.0315 0.141 Uiso 0.72(3) 1 calc PR B 1 C18A C 0.6000(10) 0.204(2) -0.1349(8) 0.087(4) Uani 0.28(3) 1 d PDU B 2 H18D H 0.6238 0.2619 -0.1527 0.130 Uiso 0.28(3) 1 calc PR B 2 H18E H 0.5791 0.2757 -0.1185 0.130 Uiso 0.28(3) 1 calc PR B 2 H18F H 0.5721 0.1397 -0.1607 0.130 Uiso 0.28(3) 1 calc PR B 2 C19A C 0.6032(12) -0.006(3) -0.0650(10) 0.109(5) Uani 0.28(3) 1 d PDU B 2 H19D H 0.6287 -0.0724 -0.0381 0.163 Uiso 0.28(3) 1 calc PR B 2 H19E H 0.5771 -0.0706 -0.0922 0.163 Uiso 0.28(3) 1 calc PR B 2 H19F H 0.5802 0.0595 -0.0486 0.163 Uiso 0.28(3) 1 calc PR B 2 C20 C 0.72239(12) 0.3614(3) -0.08652(11) 0.0648(7) Uani 1 1 d . . . H20 H 0.6909 0.4266 -0.1097 0.078 Uiso 1 1 calc R B . C21 C 0.75044(19) 0.2708(5) -0.12263(17) 0.1256(16) Uani 1 1 d . B . H21A H 0.7712 0.3422 -0.1394 0.188 Uiso 1 1 calc R . . H21B H 0.7202 0.2173 -0.1498 0.188 Uiso 1 1 calc R . . H21C H 0.7778 0.1953 -0.1016 0.188 Uiso 1 1 calc R . . C22 C 0.76601(17) 0.4702(5) -0.04999(15) 0.1211(14) Uani 1 1 d . B . H22A H 0.7980 0.4101 -0.0272 0.182 Uiso 1 1 calc R . . H22B H 0.7466 0.5282 -0.0282 0.182 Uiso 1 1 calc R . . H22C H 0.7813 0.5421 -0.0712 0.182 Uiso 1 1 calc R . . Ni2 Ni 0.011556(12) 0.24225(3) 0.141603(11) 0.04419(9) Uani 1 1 d . . . Cl2 Cl -0.05648(3) 0.10018(10) 0.08602(3) 0.0918(3) Uani 1 1 d . . . P3 P -0.04379(2) 0.36609(7) 0.18128(2) 0.04449(14) Uani 1 1 d . . . P4 P 0.08467(3) 0.15545(7) 0.11613(2) 0.04580(14) Uani 1 1 d . D . O3 O 0.00183(6) 0.47697(18) 0.22784(6) 0.0509(4) Uani 1 1 d . . . O4 O 0.14365(6) 0.25448(18) 0.15071(6) 0.0533(4) Uani 1 1 d . . . C23 C 0.05970(9) 0.4655(2) 0.22494(8) 0.0433(5) Uani 1 1 d . . . C24 C 0.07131(9) 0.3640(2) 0.18841(8) 0.0414(5) Uani 1 1 d . . . C25 C 0.13102(9) 0.3555(2) 0.18795(8) 0.0448(5) Uani 1 1 d . . . C26 C 0.17579(10) 0.4401(3) 0.22183(9) 0.0520(6) Uani 1 1 d . . . H26 H 0.2146 0.4289 0.2205 0.062 Uiso 1 1 calc R . . C27 C 0.20681(12) 0.6373(3) 0.29467(10) 0.0627(7) Uani 1 1 d . . . H27 H 0.2462 0.6266 0.2950 0.075 Uiso 1 1 calc R . . C28 C 0.19232(13) 0.7415(3) 0.32864(11) 0.0722(8) Uani 1 1 d . . . H28 H 0.2220 0.8009 0.3520 0.087 Uiso 1 1 calc R . . C29 C 0.13370(13) 0.7607(3) 0.32895(10) 0.0699(8) Uani 1 1 d . . . H29 H 0.1244 0.8340 0.3519 0.084 Uiso 1 1 calc R . . C30 C 0.08966(12) 0.6716(3) 0.29550(9) 0.0572(6) Uani 1 1 d . . . H30 H 0.0506 0.6841 0.2960 0.069 Uiso 1 1 calc R . . C31 C 0.10319(10) 0.5617(2) 0.26041(8) 0.0452(5) Uani 1 1 d . . . C32 C 0.16239(10) 0.5447(3) 0.25879(8) 0.0488(5) Uani 1 1 d . . . C33 C -0.09561(11) 0.5143(3) 0.14465(10) 0.0589(6) Uani 1 1 d . . . H33 H -0.1094 0.5743 0.1709 0.071 Uiso 1 1 calc R . . C34 C -0.06306(16) 0.6271(4) 0.11775(14) 0.1012(11) Uani 1 1 d . . . H34A H -0.0472 0.5701 0.0931 0.152 Uiso 1 1 calc R . . H34B H -0.0313 0.6766 0.1447 0.152 Uiso 1 1 calc R . . H34C H -0.0901 0.7060 0.0984 0.152 Uiso 1 1 calc R . . C35 C -0.14966(14) 0.4400(4) 0.10495(15) 0.1171(14) Uani 1 1 d . . . H35A H -0.1771 0.5210 0.0879 0.176 Uiso 1 1 calc R . . H35B H -0.1685 0.3697 0.1238 0.176 Uiso 1 1 calc R . . H35C H -0.1375 0.3825 0.0781 0.176 Uiso 1 1 calc R . . C36 C -0.08229(12) 0.2512(3) 0.21991(11) 0.0656(7) Uani 1 1 d . . . H36 H -0.1144 0.1947 0.1940 0.079 Uiso 1 1 calc R . . C37 C -0.11058(18) 0.3497(5) 0.25448(15) 0.1167(14) Uani 1 1 d . . . H37A H -0.1306 0.2820 0.2732 0.175 Uiso 1 1 calc R . . H37B H -0.1386 0.4211 0.2320 0.175 Uiso 1 1 calc R . . H37C H -0.0804 0.4083 0.2802 0.175 Uiso 1 1 calc R . . C38 C -0.03996(16) 0.1280(4) 0.25227(14) 0.1060(12) Uani 1 1 d . . . H38A H -0.0073 0.1792 0.2776 0.159 Uiso 1 1 calc R . . H38B H -0.0254 0.0640 0.2284 0.159 Uiso 1 1 calc R . . H38C H -0.0605 0.0630 0.2713 0.159 Uiso 1 1 calc R . . C39 C 0.08336(12) 0.1968(4) 0.04710(10) 0.0670(7) Uani 1 1 d U . . H39 H 0.0503 0.1390 0.0228 0.080 Uiso 1 1 calc R C 1 C40 C 0.0718(7) 0.3787(16) 0.0373(5) 0.093(3) Uani 0.76(4) 1 d PU D 1 H40A H 0.0359 0.4071 0.0453 0.139 Uiso 0.76(4) 1 calc PR D 1 H40B H 0.0682 0.4030 0.0004 0.139 Uiso 0.76(4) 1 calc PR D 1 H40C H 0.1044 0.4366 0.0603 0.139 Uiso 0.76(4) 1 calc PR D 1 C40A C 0.0522(16) 0.329(5) 0.0283(12) 0.080(5) Uani 0.24(4) 1 d PU D 2 H40D H 0.0177 0.3338 0.0408 0.120 Uiso 0.24(4) 1 calc PR D 2 H40E H 0.0402 0.3284 -0.0104 0.120 Uiso 0.24(4) 1 calc PR D 2 H40F H 0.0766 0.4199 0.0410 0.120 Uiso 0.24(4) 1 calc PR D 2 C41 C 0.14042(13) 0.1514(4) 0.03446(12) 0.0835(9) Uani 1 1 d . D . H41A H 0.1379 0.1821 -0.0017 0.125 Uiso 1 1 calc R . . H41B H 0.1460 0.0396 0.0381 0.125 Uiso 1 1 calc R . . H41C H 0.1734 0.2038 0.0591 0.125 Uiso 1 1 calc R . . C42 C 0.11063(13) -0.0449(3) 0.13123(13) 0.0852(9) Uani 1 1 d DU . . H42 H 0.1518 -0.0519 0.1302 0.102 Uiso 1 1 calc R D 1 C43 C 0.1077(9) -0.0965(18) 0.1871(4) 0.128(3) Uani 0.65(3) 1 d PDU D 1 H43A H 0.1345 -0.0337 0.2142 0.192 Uiso 0.65(3) 1 calc PR D 1 H43B H 0.1187 -0.2052 0.1926 0.192 Uiso 0.65(3) 1 calc PR D 1 H43C H 0.0680 -0.0828 0.1892 0.192 Uiso 0.65(3) 1 calc PR D 1 C44 C 0.0710(6) -0.1511(14) 0.0861(6) 0.106(3) Uani 0.65(3) 1 d PDU D 1 H44A H 0.0738 -0.1162 0.0517 0.158 Uiso 0.65(3) 1 calc PR D 1 H44B H 0.0306 -0.1444 0.0867 0.158 Uiso 0.65(3) 1 calc PR D 1 H44C H 0.0843 -0.2581 0.0919 0.158 Uiso 0.65(3) 1 calc PR D 1 C43A C 0.1252(11) -0.053(3) 0.1937(3) 0.103(4) Uani 0.35(3) 1 d PDU D 2 H43D H 0.1457 0.0413 0.2092 0.154 Uiso 0.35(3) 1 calc PR D 2 H43E H 0.1498 -0.1425 0.2069 0.154 Uiso 0.35(3) 1 calc PR D 2 H43F H 0.0890 -0.0616 0.2034 0.154 Uiso 0.35(3) 1 calc PR D 2 C44A C 0.0739(11) -0.188(2) 0.1044(10) 0.120(5) Uani 0.35(3) 1 d PDU D 2 H44D H 0.0654 -0.1803 0.0661 0.179 Uiso 0.35(3) 1 calc PR D 2 H44E H 0.0373 -0.1907 0.1138 0.179 Uiso 0.35(3) 1 calc PR D 2 H44F H 0.0959 -0.2827 0.1168 0.179 Uiso 0.35(3) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03712(15) 0.04170(16) 0.03910(15) 0.00106(12) 0.00835(11) 0.00558(11) Cl1 0.0734(4) 0.0785(4) 0.0610(4) 0.0190(3) 0.0133(3) 0.0344(4) P1 0.0390(3) 0.0410(3) 0.0412(3) -0.0039(2) 0.0090(2) 0.0065(2) P2 0.0430(3) 0.0534(3) 0.0420(3) 0.0025(3) 0.0150(3) 0.0037(3) O1 0.0467(9) 0.0522(8) 0.0379(8) -0.0011(7) 0.0108(7) 0.0132(7) O2 0.0574(10) 0.0647(10) 0.0491(9) 0.0115(8) 0.0268(8) 0.0190(8) C1 0.0370(11) 0.0386(11) 0.0425(12) -0.0034(9) 0.0097(9) 0.0007(9) C2 0.0340(11) 0.0365(10) 0.0409(11) 0.0010(9) 0.0077(9) 0.0015(8) C3 0.0434(12) 0.0441(12) 0.0458(12) 0.0051(10) 0.0185(10) 0.0047(9) C4 0.0440(12) 0.0495(13) 0.0605(14) 0.0078(11) 0.0208(11) 0.0125(10) C5 0.0507(14) 0.0515(13) 0.0658(16) 0.0116(12) 0.0129(12) 0.0133(11) C6 0.0603(16) 0.0551(15) 0.0644(16) 0.0181(13) 0.0018(13) 0.0082(12) C7 0.0714(17) 0.0592(15) 0.0460(13) 0.0098(12) 0.0050(12) 0.0035(13) C8 0.0576(14) 0.0510(13) 0.0439(12) 0.0000(11) 0.0098(11) 0.0028(11) C9 0.0396(11) 0.0369(11) 0.0433(12) 0.0005(9) 0.0069(9) -0.0020(9) C10 0.0387(11) 0.0376(11) 0.0535(13) 0.0040(10) 0.0117(10) 0.0014(9) C11 0.0401(12) 0.0673(15) 0.0527(14) -0.0055(12) 0.0128(10) 0.0018(11) C12 0.076(2) 0.089(2) 0.114(3) -0.036(2) 0.0423(18) -0.0356(17) C13 0.0649(18) 0.121(2) 0.0645(18) -0.0073(18) 0.0294(14) -0.0097(17) C14 0.0745(17) 0.0441(13) 0.0564(14) -0.0096(11) 0.0171(13) 0.0033(12) C15 0.109(3) 0.076(2) 0.102(3) -0.0267(18) 0.033(2) -0.0363(19) C16 0.127(3) 0.0558(17) 0.100(2) -0.0074(17) 0.021(2) 0.0364(18) C17 0.0643(16) 0.0883(19) 0.0667(16) -0.0330(14) 0.0242(13) -0.0074(14) C18 0.056(4) 0.144(6) 0.123(5) -0.065(4) -0.014(4) 0.003(4) C19 0.092(5) 0.105(4) 0.103(4) -0.044(2) 0.056(4) -0.057(4) C18A 0.035(7) 0.119(8) 0.086(7) -0.063(4) -0.013(6) 0.000(6) C19A 0.083(10) 0.142(10) 0.119(9) -0.065(6) 0.057(8) -0.060(8) C20 0.0617(16) 0.0747(17) 0.0635(16) 0.0242(14) 0.0267(13) 0.0088(13) C21 0.164(4) 0.115(3) 0.147(3) 0.034(3) 0.123(3) 0.027(3) C22 0.114(3) 0.126(3) 0.119(3) 0.032(3) 0.029(2) -0.055(2) Ni2 0.03842(16) 0.04659(17) 0.04605(17) -0.00676(12) 0.00991(12) -0.00478(12) Cl2 0.0534(4) 0.1067(6) 0.1095(6) -0.0566(5) 0.0147(4) -0.0219(4) P3 0.0414(3) 0.0490(3) 0.0445(3) -0.0022(3) 0.0147(2) -0.0053(2) P4 0.0426(3) 0.0432(3) 0.0513(3) -0.0024(3) 0.0131(3) -0.0004(2) O3 0.0481(9) 0.0587(9) 0.0492(9) -0.0118(7) 0.0193(7) -0.0096(7) O4 0.0390(8) 0.0631(10) 0.0568(9) -0.0100(8) 0.0123(7) 0.0001(7) C23 0.0419(12) 0.0479(12) 0.0398(11) 0.0051(10) 0.0113(9) -0.0066(10) C24 0.0439(12) 0.0415(11) 0.0364(11) 0.0021(9) 0.0079(9) -0.0031(9) C25 0.0407(12) 0.0482(12) 0.0437(12) 0.0022(10) 0.0095(9) -0.0005(10) C26 0.0373(12) 0.0601(14) 0.0549(14) 0.0018(12) 0.0073(10) -0.0015(10) C27 0.0563(15) 0.0634(16) 0.0595(15) 0.0004(13) 0.0027(12) -0.0127(12) C28 0.076(2) 0.0697(18) 0.0617(17) -0.0131(14) 0.0063(14) -0.0220(15) C29 0.087(2) 0.0670(17) 0.0570(16) -0.0183(13) 0.0226(14) -0.0218(15) C30 0.0662(16) 0.0588(15) 0.0490(14) -0.0056(12) 0.0207(12) -0.0113(12) C31 0.0550(13) 0.0450(12) 0.0340(11) 0.0032(9) 0.0104(10) -0.0069(10) C32 0.0478(13) 0.0506(13) 0.0424(12) 0.0065(10) 0.0042(10) -0.0071(10) C33 0.0578(15) 0.0601(15) 0.0600(15) -0.0014(12) 0.0190(12) 0.0101(12) C34 0.125(3) 0.096(2) 0.102(3) 0.047(2) 0.062(2) 0.039(2) C35 0.081(2) 0.114(3) 0.118(3) -0.013(2) -0.032(2) 0.032(2) C36 0.0667(17) 0.0705(18) 0.0636(16) 0.0020(13) 0.0251(13) -0.0229(13) C37 0.143(3) 0.128(3) 0.117(3) -0.011(2) 0.097(3) -0.031(3) C38 0.107(3) 0.108(3) 0.094(2) 0.045(2) 0.014(2) -0.023(2) C39 0.0621(17) 0.0897(19) 0.0489(14) -0.0082(14) 0.0158(12) 0.0043(14) C40 0.101(6) 0.097(5) 0.089(5) 0.039(4) 0.041(4) 0.032(4) C40A 0.095(11) 0.100(10) 0.051(8) 0.028(8) 0.029(8) 0.003(8) C41 0.085(2) 0.103(2) 0.0759(19) -0.0110(17) 0.0441(17) 0.0013(18) C42 0.0767(19) 0.0475(15) 0.143(3) 0.0144(16) 0.0506(19) 0.0108(13) C43 0.146(9) 0.087(6) 0.166(4) 0.070(4) 0.067(5) 0.012(6) C44 0.118(5) 0.024(4) 0.193(6) -0.009(4) 0.074(5) -0.016(4) C43A 0.095(9) 0.067(8) 0.154(4) 0.079(5) 0.048(6) 0.013(6) C44A 0.117(8) 0.036(7) 0.220(10) 0.019(7) 0.071(8) -0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C2 1.8758(19) . ? Ni1 P2 2.1459(6) . ? Ni1 P1 2.1576(6) . ? Ni1 Cl1 2.1850(6) . ? P1 O1 1.6539(14) . ? P1 C11 1.820(2) . ? P1 C14 1.821(2) . ? P2 O2 1.6466(16) . ? P2 C20 1.816(2) . ? P2 C17 1.822(3) . ? O1 C1 1.393(2) . ? O2 C3 1.395(2) . ? C1 C2 1.377(3) . ? C1 C9 1.410(3) . ? C2 C3 1.412(3) . ? C3 C4 1.354(3) . ? C4 C10 1.415(3) . ? C5 C6 1.350(3) . ? C5 C10 1.413(3) . ? C6 C7 1.396(3) . ? C7 C8 1.362(3) . ? C8 C9 1.407(3) . ? C9 C10 1.418(3) . ? C11 C13 1.515(3) . ? C11 C12 1.522(4) . ? C14 C15 1.518(4) . ? C14 C16 1.522(3) . ? C17 C18 1.531(5) . ? C17 C19A 1.533(7) . ? C17 C19 1.550(5) . ? C17 C18A 1.556(7) . ? C20 C22 1.498(4) . ? C20 C21 1.506(4) . ? Ni2 C24 1.881(2) . ? Ni2 P4 2.1481(6) . ? Ni2 P3 2.1568(6) . ? Ni2 Cl2 2.1834(7) . ? P3 O3 1.6584(15) . ? P3 C33 1.819(2) . ? P3 C36 1.820(2) . ? P4 O4 1.6500(15) . ? P4 C42 1.814(3) . ? P4 C39 1.817(3) . ? O3 C23 1.391(2) . ? O4 C25 1.389(3) . ? C23 C24 1.367(3) . ? C23 C31 1.421(3) . ? C24 C25 1.413(3) . ? C25 C26 1.366(3) . ? C26 C32 1.409(3) . ? C27 C28 1.362(4) . ? C27 C32 1.420(3) . ? C28 C29 1.394(4) . ? C29 C30 1.372(3) . ? C30 C31 1.405(3) . ? C31 C32 1.416(3) . ? C33 C34 1.519(4) . ? C33 C35 1.523(4) . ? C36 C37 1.516(4) . ? C36 C38 1.520(4) . ? C39 C40A 1.36(3) . ? C39 C41 1.524(4) . ? C39 C40 1.577(12) . ? C42 C43 1.535(6) . ? C42 C44A 1.538(7) . ? C42 C44 1.557(6) . ? C42 C43A 1.557(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ni1 P2 82.10(6) . . ? C2 Ni1 P1 82.49(6) . . ? P2 Ni1 P1 162.93(3) . . ? C2 Ni1 Cl1 176.39(6) . . ? P2 Ni1 Cl1 96.93(3) . . ? P1 Ni1 Cl1 98.89(2) . . ? O1 P1 C11 102.48(10) . . ? O1 P1 C14 101.07(9) . . ? C11 P1 C14 107.27(11) . . ? O1 P1 Ni1 105.69(5) . . ? C11 P1 Ni1 115.83(8) . . ? C14 P1 Ni1 121.64(9) . . ? O2 P2 C20 102.40(10) . . ? O2 P2 C17 102.59(11) . . ? C20 P2 C17 107.84(13) . . ? O2 P2 Ni1 106.41(6) . . ? C20 P2 Ni1 119.78(9) . . ? C17 P2 Ni1 115.53(9) . . ? C1 O1 P1 111.45(12) . . ? C3 O2 P2 111.75(12) . . ? C2 C1 O1 118.12(17) . . ? C2 C1 C9 124.16(18) . . ? O1 C1 C9 117.72(17) . . ? C1 C2 C3 115.55(18) . . ? C1 C2 Ni1 122.16(15) . . ? C3 C2 Ni1 122.29(15) . . ? C4 C3 O2 119.51(18) . . ? C4 C3 C2 124.15(19) . . ? O2 C3 C2 116.34(17) . . ? C3 C4 C10 119.00(19) . . ? C6 C5 C10 121.4(2) . . ? C5 C6 C7 120.5(2) . . ? C8 C7 C6 120.1(2) . . ? C7 C8 C9 120.8(2) . . ? C8 C9 C1 123.71(19) . . ? C8 C9 C10 119.11(19) . . ? C1 C9 C10 117.17(18) . . ? C5 C10 C4 122.1(2) . . ? C5 C10 C9 117.9(2) . . ? C4 C10 C9 119.94(18) . . ? C13 C11 C12 112.3(2) . . ? C13 C11 P1 113.71(17) . . ? C12 C11 P1 109.36(17) . . ? C15 C14 C16 112.4(3) . . ? C15 C14 P1 109.12(18) . . ? C16 C14 P1 111.68(18) . . ? C18 C17 C19A 87.1(9) . . ? C18 C17 C19 111.0(4) . . ? C19A C17 C18A 110.1(7) . . ? C19 C17 C18A 133.8(8) . . ? C18 C17 P2 113.5(5) . . ? C19A C17 P2 115.6(10) . . ? C19 C17 P2 107.2(4) . . ? C18A C17 P2 102.4(9) . . ? C22 C20 C21 111.4(3) . . ? C22 C20 P2 108.84(19) . . ? C21 C20 P2 114.4(2) . . ? C24 Ni2 P4 82.57(7) . . ? C24 Ni2 P3 82.31(7) . . ? P4 Ni2 P3 164.88(3) . . ? C24 Ni2 Cl2 178.65(7) . . ? P4 Ni2 Cl2 96.17(3) . . ? P3 Ni2 Cl2 98.94(3) . . ? O3 P3 C33 100.48(10) . . ? O3 P3 C36 103.00(10) . . ? C33 P3 C36 107.03(12) . . ? O3 P3 Ni2 105.75(6) . . ? C33 P3 Ni2 119.74(8) . . ? C36 P3 Ni2 117.97(9) . . ? O4 P4 C42 100.57(11) . . ? O4 P4 C39 101.99(11) . . ? C42 P4 C39 107.64(14) . . ? O4 P4 Ni2 106.37(6) . . ? C42 P4 Ni2 120.43(10) . . ? C39 P4 Ni2 116.86(9) . . ? C23 O3 P3 111.04(12) . . ? C25 O4 P4 112.16(13) . . ? C24 C23 O3 118.60(18) . . ? C24 C23 C31 124.1(2) . . ? O3 C23 C31 117.30(18) . . ? C23 C24 C25 116.02(19) . . ? C23 C24 Ni2 122.15(16) . . ? C25 C24 Ni2 121.83(16) . . ? C26 C25 O4 119.49(19) . . ? C26 C25 C24 123.6(2) . . ? O4 C25 C24 116.94(18) . . ? C25 C26 C32 119.1(2) . . ? C28 C27 C32 120.6(3) . . ? C27 C28 C29 121.0(2) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 120.3(2) . . ? C30 C31 C32 119.9(2) . . ? C30 C31 C23 123.1(2) . . ? C32 C31 C23 117.0(2) . . ? C26 C32 C31 120.16(19) . . ? C26 C32 C27 121.8(2) . . ? C31 C32 C27 118.0(2) . . ? C34 C33 C35 112.7(3) . . ? C34 C33 P3 108.99(18) . . ? C35 C33 P3 111.66(19) . . ? C37 C36 C38 112.6(3) . . ? C37 C36 P3 113.9(2) . . ? C38 C36 P3 108.8(2) . . ? C40A C39 C41 123.5(14) . . ? C41 C39 C40 109.6(6) . . ? C40A C39 P4 111.6(13) . . ? C41 C39 P4 113.6(2) . . ? C40 C39 P4 107.5(4) . . ? C43 C42 C44A 91.5(8) . . ? C43 C42 C44 111.3(4) . . ? C44A C42 C43A 111.2(7) . . ? C44 C42 C43A 131.4(7) . . ? C43 C42 P4 111.6(6) . . ? C44A C42 P4 122.4(11) . . ? C44 C42 P4 106.9(6) . . ? C43A C42 P4 102.9(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.450 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.062 #============================================================================== data_compound-2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H33 Cl O2 P2 Pd' _chemical_formula_sum 'C22 H33 Cl O2 P2 Pd' _chemical_formula_weight 533.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.216(4) _cell_length_b 8.2920(9) _cell_length_c 19.034(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.934(2) _cell_angle_gamma 90.00 _cell_volume 5108.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9541 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.26 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.6899 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker Smart APEX AXS CCD area detector 01-670 ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 20415 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4664 _reflns_number_gt 3655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _solved_by 'Simon Hernandez-Ortega' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4664 _refine_ls_number_parameters 312 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.146447(7) -0.03702(3) 0.387907(11) 0.05034(9) Uani 1 1 d . A . Cl Cl 0.16921(3) -0.17741(11) 0.50166(4) 0.0852(3) Uani 1 1 d . . . P2 P 0.19431(3) -0.12064(10) 0.33666(4) 0.0576(2) Uani 1 1 d . . . O1 O 0.06864(6) 0.1795(3) 0.32213(11) 0.0720(6) Uani 1 1 d . A . O2 O 0.18273(7) -0.0235(2) 0.25743(10) 0.0663(6) Uani 1 1 d . . . C1 C 0.09171(9) 0.1728(4) 0.27382(14) 0.0528(7) Uani 1 1 d . . . C2 C 0.12647(9) 0.0799(3) 0.29215(14) 0.0478(7) Uani 1 1 d . . . C3 C 0.14770(9) 0.0722(3) 0.23975(14) 0.0487(7) Uani 1 1 d . . . C4 C 0.13526(9) 0.1531(3) 0.17441(14) 0.0525(7) Uani 1 1 d . . . H4 H 0.1500 0.1438 0.1413 0.063 Uiso 1 1 calc R . . C5 C 0.08595(10) 0.3393(4) 0.09004(15) 0.0643(8) Uani 1 1 d . . . H5 H 0.1001 0.3310 0.0558 0.077 Uiso 1 1 calc R . . C6 C 0.05230(12) 0.4361(4) 0.07488(19) 0.0818(11) Uani 1 1 d . . . H6 H 0.0436 0.4935 0.0305 0.098 Uiso 1 1 calc R . . C7 C 0.03080(12) 0.4502(5) 0.1250(2) 0.0917(12) Uani 1 1 d . . . H7 H 0.0078 0.5171 0.1140 0.110 Uiso 1 1 calc R . . C8 C 0.04299(10) 0.3670(4) 0.19060(18) 0.0797(10) Uani 1 1 d . . . H8 H 0.0285 0.3782 0.2240 0.096 Uiso 1 1 calc R . . C9 C 0.07749(8) 0.2643(3) 0.20732(15) 0.0545(7) Uani 1 1 d . . . C10 C 0.09993(9) 0.2509(3) 0.15697(14) 0.0502(7) Uani 1 1 d . . . P1 P 0.08994(3) 0.08305(11) 0.40081(5) 0.0692(3) Uani 1 1 d DU . . C11 C 0.0506(2) -0.0665(10) 0.4013(6) 0.126(3) Uani 0.743(17) 1 d PDU A 1 H11 H 0.0584 -0.1128 0.4513 0.151 Uiso 0.743(17) 1 calc PR A 1 C12 C 0.0502(3) -0.2027(9) 0.3479(6) 0.162(4) Uani 0.743(17) 1 d PDU A 1 H12A H 0.0766 -0.2558 0.3634 0.243 Uiso 0.743(17) 1 calc PR A 1 H12B H 0.0448 -0.1599 0.2988 0.243 Uiso 0.743(17) 1 calc PR A 1 H12C H 0.0290 -0.2787 0.3478 0.243 Uiso 0.743(17) 1 calc PR A 1 C13 C 0.0077(2) -0.0021(14) 0.3836(8) 0.159(4) Uani 0.743(17) 1 d PDU A 1 H13A H 0.0071 0.0767 0.4201 0.238 Uiso 0.743(17) 1 calc PR A 1 H13B H -0.0108 -0.0888 0.3840 0.238 Uiso 0.743(17) 1 calc PR A 1 H13C H -0.0006 0.0471 0.3354 0.238 Uiso 0.743(17) 1 calc PR A 1 C14 C 0.0922(3) 0.2409(9) 0.4686(4) 0.095(2) Uani 0.743(17) 1 d PDU A 1 H14 H 0.0646 0.2879 0.4572 0.114 Uiso 0.743(17) 1 calc PR A 1 C15 C 0.1053(4) 0.1768(14) 0.5477(3) 0.149(4) Uani 0.743(17) 1 d PDU A 1 H15A H 0.0897 0.0816 0.5495 0.223 Uiso 0.743(17) 1 calc PR A 1 H15B H 0.1002 0.2574 0.5800 0.223 Uiso 0.743(17) 1 calc PR A 1 H15C H 0.1342 0.1511 0.5637 0.223 Uiso 0.743(17) 1 calc PR A 1 C16 C 0.1207(4) 0.3690(11) 0.4571(6) 0.124(3) Uani 0.743(17) 1 d PDU A 1 H16A H 0.1123 0.3983 0.4055 0.186 Uiso 0.743(17) 1 calc PR A 1 H16B H 0.1485 0.3283 0.4721 0.186 Uiso 0.743(17) 1 calc PR A 1 H16C H 0.1196 0.4622 0.4863 0.186 Uiso 0.743(17) 1 calc PR A 1 C11A C 0.0500(5) -0.023(2) 0.4273(14) 0.134(5) Uani 0.257(17) 1 d PDU A 2 H11A H 0.0626 -0.0615 0.4784 0.161 Uiso 0.257(17) 1 calc PR A 2 C12A C 0.0362(7) -0.169(2) 0.3787(19) 0.156(6) Uani 0.257(17) 1 d PDU A 2 H12D H 0.0598 -0.2331 0.3802 0.234 Uiso 0.257(17) 1 calc PR A 2 H12E H 0.0223 -0.1350 0.3285 0.234 Uiso 0.257(17) 1 calc PR A 2 H12F H 0.0176 -0.2314 0.3962 0.234 Uiso 0.257(17) 1 calc PR A 2 C13A C 0.0136(6) 0.079(4) 0.4255(19) 0.142(6) Uani 0.257(17) 1 d PDU A 2 H13D H 0.0227 0.1704 0.4573 0.213 Uiso 0.257(17) 1 calc PR A 2 H13E H -0.0053 0.0163 0.4423 0.213 Uiso 0.257(17) 1 calc PR A 2 H13F H -0.0001 0.1147 0.3756 0.213 Uiso 0.257(17) 1 calc PR A 2 C14A C 0.1048(7) 0.2555(18) 0.4641(9) 0.092(4) Uani 0.257(17) 1 d PDU A 2 H14A H 0.0798 0.3163 0.4613 0.111 Uiso 0.257(17) 1 calc PR A 2 C15A C 0.1244(7) 0.198(3) 0.5432(7) 0.112(5) Uani 0.257(17) 1 d PDU A 2 H15D H 0.1055 0.1290 0.5567 0.169 Uiso 0.257(17) 1 calc PR A 2 H15E H 0.1311 0.2891 0.5760 0.169 Uiso 0.257(17) 1 calc PR A 2 H15F H 0.1492 0.1391 0.5472 0.169 Uiso 0.257(17) 1 calc PR A 2 C16A C 0.1348(9) 0.369(2) 0.4458(14) 0.100(6) Uani 0.257(17) 1 d PDU A 2 H16D H 0.1233 0.4040 0.3951 0.150 Uiso 0.257(17) 1 calc PR A 2 H16E H 0.1604 0.3141 0.4524 0.150 Uiso 0.257(17) 1 calc PR A 2 H16F H 0.1396 0.4610 0.4781 0.150 Uiso 0.257(17) 1 calc PR A 2 C17 C 0.19284(14) -0.3292(4) 0.3076(2) 0.0894(12) Uani 1 1 d . . . H17 H 0.2092 -0.3396 0.2741 0.107 Uiso 1 1 calc R . . C18 C 0.14859(17) -0.3739(6) 0.2653(2) 0.1306(18) Uani 1 1 d . . . H18A H 0.1475 -0.4837 0.2488 0.196 Uiso 1 1 calc R . . H18B H 0.1382 -0.3041 0.2231 0.196 Uiso 1 1 calc R . . H18C H 0.1320 -0.3623 0.2972 0.196 Uiso 1 1 calc R . . C19 C 0.21147(16) -0.4388(4) 0.3744(3) 0.1189(17) Uani 1 1 d . . . H19A H 0.1988 -0.4165 0.4116 0.178 Uiso 1 1 calc R . . H19B H 0.2407 -0.4195 0.3946 0.178 Uiso 1 1 calc R . . H19C H 0.2067 -0.5494 0.3592 0.178 Uiso 1 1 calc R . . C20 C 0.24776(11) -0.0663(4) 0.38030(19) 0.0746(10) Uani 1 1 d . . . H20 H 0.2583 -0.1319 0.4254 0.089 Uiso 1 1 calc R . . C21 C 0.27490(13) -0.1019(6) 0.3324(2) 0.1140(16) Uani 1 1 d . . . H21A H 0.2632 -0.0514 0.2847 0.171 Uiso 1 1 calc R . . H21B H 0.2764 -0.2163 0.3259 0.171 Uiso 1 1 calc R . . H21C H 0.3022 -0.0602 0.3563 0.171 Uiso 1 1 calc R . . C22 C 0.25072(14) 0.1091(5) 0.4048(3) 0.1269(16) Uani 1 1 d . . . H22A H 0.2792 0.1372 0.4285 0.190 Uiso 1 1 calc R . . H22B H 0.2357 0.1240 0.4390 0.190 Uiso 1 1 calc R . . H22C H 0.2391 0.1769 0.3622 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.05890(16) 0.05188(15) 0.04489(14) 0.00777(10) 0.02328(10) 0.01115(11) Cl 0.1019(7) 0.0991(7) 0.0645(5) 0.0346(5) 0.0403(5) 0.0411(6) P2 0.0716(6) 0.0520(5) 0.0573(5) 0.0086(4) 0.0321(4) 0.0179(4) O1 0.0597(13) 0.0992(17) 0.0670(13) 0.0310(12) 0.0341(11) 0.0283(12) O2 0.0760(15) 0.0780(14) 0.0550(12) 0.0145(10) 0.0353(11) 0.0280(12) C1 0.0467(17) 0.0629(19) 0.0516(17) 0.0061(14) 0.0199(14) 0.0014(15) C2 0.0524(18) 0.0505(17) 0.0416(15) 0.0029(12) 0.0168(13) 0.0002(13) C3 0.0525(18) 0.0516(18) 0.0440(16) 0.0009(12) 0.0185(13) 0.0034(13) C4 0.062(2) 0.0572(18) 0.0434(16) -0.0004(13) 0.0233(14) -0.0047(15) C5 0.067(2) 0.071(2) 0.0516(18) 0.0111(15) 0.0154(15) -0.0084(18) C6 0.080(3) 0.090(3) 0.070(2) 0.0348(19) 0.016(2) 0.008(2) C7 0.078(3) 0.102(3) 0.093(3) 0.040(2) 0.023(2) 0.032(2) C8 0.065(2) 0.102(3) 0.075(2) 0.027(2) 0.0267(18) 0.021(2) C9 0.0459(17) 0.0601(18) 0.0532(17) 0.0088(14) 0.0102(13) 0.0013(14) C10 0.0485(17) 0.0538(17) 0.0443(16) 0.0031(13) 0.0094(13) -0.0088(14) P1 0.0685(6) 0.0860(6) 0.0667(5) 0.0287(5) 0.0407(5) 0.0246(5) C11 0.088(4) 0.143(6) 0.180(7) 0.073(5) 0.090(4) 0.018(4) C12 0.105(6) 0.141(6) 0.265(10) 0.027(6) 0.095(6) -0.041(5) C13 0.108(6) 0.171(8) 0.230(10) 0.051(7) 0.099(6) 0.032(5) C14 0.135(6) 0.111(4) 0.068(3) 0.029(3) 0.071(3) 0.070(4) C15 0.223(9) 0.173(7) 0.074(4) 0.040(4) 0.082(5) 0.113(7) C16 0.173(9) 0.105(5) 0.106(5) -0.029(4) 0.063(5) 0.035(5) C11A 0.083(7) 0.153(9) 0.201(10) 0.050(8) 0.094(7) 0.023(7) C12A 0.083(10) 0.168(12) 0.247(13) 0.049(11) 0.095(9) -0.018(9) C13A 0.073(9) 0.177(14) 0.218(15) 0.042(12) 0.106(9) 0.041(9) C14A 0.146(9) 0.100(7) 0.069(6) 0.021(6) 0.087(6) 0.059(7) C15A 0.179(12) 0.123(9) 0.071(7) 0.012(7) 0.090(8) 0.059(10) C16A 0.163(14) 0.072(9) 0.089(10) -0.022(7) 0.073(9) 0.004(10) C17 0.134(4) 0.059(2) 0.093(3) -0.010(2) 0.061(3) 0.012(2) C18 0.181(5) 0.092(3) 0.118(4) -0.040(3) 0.048(4) -0.030(3) C19 0.171(5) 0.054(2) 0.147(4) 0.025(2) 0.073(4) 0.029(3) C20 0.066(2) 0.081(3) 0.079(2) 0.0266(18) 0.0271(18) 0.0226(19) C21 0.083(3) 0.147(4) 0.132(4) 0.059(3) 0.062(3) 0.041(3) C22 0.092(4) 0.093(3) 0.176(5) -0.014(3) 0.017(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C2 1.980(2) . ? Pd P1 2.2580(9) . ? Pd P2 2.2696(8) . ? Pd Cl 2.3570(8) . ? P2 O2 1.6408(19) . ? P2 C20 1.803(4) . ? P2 C17 1.811(3) . ? O1 C1 1.394(3) . ? O1 P1 1.645(2) . ? O2 C3 1.385(3) . ? C1 C2 1.364(4) . ? C1 C9 1.420(4) . ? C2 C3 1.413(4) . ? C3 C4 1.354(3) . ? C4 C10 1.404(4) . ? C5 C6 1.356(4) . ? C5 C10 1.412(4) . ? C6 C7 1.387(5) . ? C7 C8 1.367(4) . ? C8 C9 1.406(4) . ? C9 C10 1.413(4) . ? P1 C14 1.822(5) . ? P1 C11A 1.828(8) . ? P1 C14A 1.832(8) . ? P1 C11 1.833(5) . ? C11 C13 1.492(6) . ? C11 C12 1.516(6) . ? C14 C16 1.506(6) . ? C14 C15 1.521(5) . ? C11A C13A 1.498(8) . ? C11A C12A 1.501(8) . ? C14A C16A 1.514(8) . ? C14A C15A 1.514(8) . ? C17 C18 1.512(6) . ? C17 C19 1.525(5) . ? C20 C22 1.521(5) . ? C20 C21 1.527(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd P1 80.34(8) . . ? C2 Pd P2 80.54(8) . . ? P1 Pd P2 160.78(3) . . ? C2 Pd Cl 179.15(8) . . ? P1 Pd Cl 99.05(3) . . ? P2 Pd Cl 100.05(3) . . ? O2 P2 C20 101.96(14) . . ? O2 P2 C17 102.31(14) . . ? C20 P2 C17 107.62(18) . . ? O2 P2 Pd 104.61(8) . . ? C20 P2 Pd 119.41(12) . . ? C17 P2 Pd 118.07(14) . . ? C1 O1 P1 113.73(18) . . ? C3 O2 P2 115.88(16) . . ? C2 C1 O1 119.2(2) . . ? C2 C1 C9 123.2(2) . . ? O1 C1 C9 117.6(2) . . ? C1 C2 C3 116.8(2) . . ? C1 C2 Pd 121.58(19) . . ? C3 C2 Pd 121.7(2) . . ? C4 C3 O2 119.7(2) . . ? C4 C3 C2 123.1(3) . . ? O2 C3 C2 117.2(2) . . ? C3 C4 C10 119.6(2) . . ? C6 C5 C10 121.0(3) . . ? C5 C6 C7 120.5(3) . . ? C8 C7 C6 120.9(3) . . ? C7 C8 C9 119.8(3) . . ? C8 C9 C10 119.7(3) . . ? C8 C9 C1 123.0(3) . . ? C10 C9 C1 117.3(3) . . ? C4 C10 C5 121.8(3) . . ? C4 C10 C9 120.0(2) . . ? C5 C10 C9 118.1(3) . . ? O1 P1 C14 101.5(3) . . ? O1 P1 C11A 109.6(7) . . ? C14 P1 C11A 90.9(6) . . ? O1 P1 C14A 99.5(7) . . ? C11A P1 C14A 105.6(8) . . ? O1 P1 C11 103.0(3) . . ? C14 P1 C11 110.2(3) . . ? C14A P1 C11 125.0(5) . . ? O1 P1 Pd 104.92(7) . . ? C14 P1 Pd 123.5(3) . . ? C11A P1 Pd 124.1(6) . . ? C14A P1 Pd 110.5(7) . . ? C11 P1 Pd 111.0(3) . . ? C13 C11 C12 108.8(6) . . ? C13 C11 P1 115.3(5) . . ? C12 C11 P1 110.3(4) . . ? C16 C14 C15 113.2(7) . . ? C16 C14 P1 106.5(5) . . ? C15 C14 P1 112.4(4) . . ? C13A C11A C12A 110.2(10) . . ? C13A C11A P1 114.4(8) . . ? C12A C11A P1 109.4(8) . . ? C16A C14A C15A 108.1(10) . . ? C16A C14A P1 113.5(8) . . ? C15A C14A P1 110.3(8) . . ? C18 C17 C19 111.9(4) . . ? C18 C17 P2 108.7(3) . . ? C19 C17 P2 110.6(3) . . ? C22 C20 C21 112.0(3) . . ? C22 C20 P2 109.7(2) . . ? C21 C20 P2 113.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.661 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.067 #============================================================================== data_compound-4a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl Ni O2 P2 Ru, F6 P' _chemical_formula_sum 'C54 H76 Cl2 F12 Ni2 O4 P6 Ru2' _chemical_formula_weight 1593.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.787(1) _cell_length_b 13.557(1) _cell_length_c 27.926(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.041(1) _cell_angle_gamma 90.00 _cell_volume 6355.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 11128 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6853 _exptl_absorpt_correction_T_max 0.7915 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46108 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 30.03 _reflns_number_total 18312 _reflns_number_gt 17483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Crystal were found to be twinned ; twin fraction 0.61/0.39 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+6.1946P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18312 _refine_ls_number_parameters 756 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.52358(2) 0.15111(3) 0.185866(13) 0.02604(7) Uani 1 1 d . . . Ru1 Ru 0.830731(14) 0.207172(15) 0.089048(8) 0.02390(5) Uani 1 1 d . . . Cl1 Cl 0.43215(5) 0.16660(7) 0.24127(3) 0.04195(19) Uani 1 1 d . . . P1 P 0.44910(4) 0.17198(6) 0.12328(3) 0.02668(14) Uani 1 1 d . . . P2 P 0.62326(5) 0.13673(6) 0.23428(3) 0.02678(14) Uani 1 1 d . . . O1 O 0.50955(13) 0.16622(18) 0.07680(7) 0.0316(5) Uani 1 1 d . . . O2 O 0.70014(12) 0.10341(16) 0.19989(7) 0.0285(4) Uani 1 1 d . . . C1 C 0.60304(17) 0.1342(2) 0.13965(10) 0.0252(5) Uani 1 1 d . . . C2 C 0.58650(16) 0.1444(2) 0.08916(10) 0.0248(5) Uani 1 1 d . . . C3 C 0.64299(17) 0.1352(2) 0.05434(10) 0.0277(5) Uani 1 1 d . . . H3 H 0.6297 0.1449 0.0216 0.033 Uiso 1 1 calc R . . C4 C 0.72226(18) 0.1107(2) 0.06816(10) 0.0262(5) Uani 1 1 d . . . C5 C 0.74209(16) 0.0966(2) 0.11819(10) 0.0243(5) Uani 1 1 d . . . C6 C 0.67954(17) 0.11193(19) 0.15231(9) 0.0245(5) Uani 1 1 d . . . C7 C 0.78508(19) 0.1038(2) 0.03389(11) 0.0302(6) Uani 1 1 d . . . H7 H 0.7743 0.1192 0.0013 0.036 Uiso 1 1 calc R . . C8 C 0.86278(19) 0.0748(2) 0.04718(11) 0.0308(6) Uani 1 1 d . . . H8 H 0.9030 0.0669 0.0236 0.037 Uiso 1 1 calc R . . C9 C 0.88008(18) 0.0577(2) 0.09589(12) 0.0305(6) Uani 1 1 d . . . H9 H 0.9318 0.0360 0.1048 0.037 Uiso 1 1 calc R . . C10 C 0.82202(17) 0.07229(18) 0.13145(10) 0.0257(5) Uani 1 1 d . . . H10 H 0.8359 0.0660 0.1643 0.031 Uiso 1 1 calc R . . C11 C 0.4074(2) 0.2959(2) 0.11815(12) 0.0318(6) Uani 1 1 d . . . H11 H 0.3692 0.3055 0.1452 0.038 Uiso 1 1 calc R . . C12 C 0.4751(2) 0.3707(3) 0.12427(14) 0.0422(8) Uani 1 1 d . . . H12A H 0.5140 0.3620 0.0985 0.063 Uiso 1 1 calc R . . H12B H 0.5013 0.3601 0.1552 0.063 Uiso 1 1 calc R . . H12C H 0.4534 0.4377 0.1230 0.063 Uiso 1 1 calc R . . C13 C 0.3625(3) 0.3146(3) 0.07164(16) 0.0544(11) Uani 1 1 d . . . H13A H 0.3424 0.3825 0.0714 0.082 Uiso 1 1 calc R . . H13B H 0.3177 0.2685 0.0692 0.082 Uiso 1 1 calc R . . H13C H 0.3985 0.3048 0.0444 0.082 Uiso 1 1 calc R . . C14 C 0.37350(19) 0.0819(2) 0.10583(12) 0.0336(6) Uani 1 1 d . . . H14 H 0.3493 0.1036 0.0748 0.040 Uiso 1 1 calc R . . C15 C 0.4140(3) -0.0177(3) 0.09805(19) 0.0575(11) Uani 1 1 d . . . H15A H 0.4345 -0.0423 0.1286 0.086 Uiso 1 1 calc R . . H15B H 0.4581 -0.0099 0.0754 0.086 Uiso 1 1 calc R . . H15C H 0.3753 -0.0647 0.0851 0.086 Uiso 1 1 calc R . . C16 C 0.3080(2) 0.0753(3) 0.14293(16) 0.0512(10) Uani 1 1 d . . . H16A H 0.2686 0.0261 0.1328 0.077 Uiso 1 1 calc R . . H16B H 0.2821 0.1397 0.1462 0.077 Uiso 1 1 calc R . . H16C H 0.3309 0.0557 0.1738 0.077 Uiso 1 1 calc R . . C17 C 0.6634(2) 0.2451(3) 0.26449(12) 0.0366(6) Uani 1 1 d . . . H17 H 0.7162 0.2269 0.2786 0.044 Uiso 1 1 calc R . . C18 C 0.6768(3) 0.3280(3) 0.22833(16) 0.0568(11) Uani 1 1 d . . . H18A H 0.6253 0.3506 0.2159 0.085 Uiso 1 1 calc R . . H18B H 0.7096 0.3036 0.2018 0.085 Uiso 1 1 calc R . . H18C H 0.7041 0.3831 0.2441 0.085 Uiso 1 1 calc R . . C19 C 0.6089(3) 0.2783(3) 0.30507(14) 0.0521(10) Uani 1 1 d . . . H19A H 0.6329 0.3348 0.3216 0.078 Uiso 1 1 calc R . . H19B H 0.6017 0.2240 0.3278 0.078 Uiso 1 1 calc R . . H19C H 0.5570 0.2976 0.2919 0.078 Uiso 1 1 calc R . . C20 C 0.6195(2) 0.0379(2) 0.27839(11) 0.0323(6) Uani 1 1 d . . . H20 H 0.5754 0.0536 0.3012 0.039 Uiso 1 1 calc R . . C21 C 0.5976(3) -0.0580(3) 0.25277(14) 0.0565(11) Uani 1 1 d . . . H21A H 0.6411 -0.0772 0.2313 0.085 Uiso 1 1 calc R . . H21B H 0.5488 -0.0480 0.2341 0.085 Uiso 1 1 calc R . . H21C H 0.5888 -0.1101 0.2765 0.085 Uiso 1 1 calc R . . C22 C 0.6965(3) 0.0283(3) 0.30758(14) 0.0496(9) Uani 1 1 d . . . H22A H 0.6906 -0.0249 0.3310 0.074 Uiso 1 1 calc R . . H22B H 0.7071 0.0905 0.3243 0.074 Uiso 1 1 calc R . . H22C H 0.7409 0.0133 0.2861 0.074 Uiso 1 1 calc R . . C23 C 0.8651(3) 0.3207(2) 0.13951(13) 0.0437(9) Uani 1 1 d . . . H23 H 0.8679 0.3103 0.1731 0.052 Uiso 1 1 calc R . . C24 C 0.7979(2) 0.3542(2) 0.11382(14) 0.0412(8) Uani 1 1 d . . . H24 H 0.7477 0.3708 0.1273 0.049 Uiso 1 1 calc R . . C25 C 0.8179(2) 0.3591(2) 0.06456(13) 0.0357(7) Uani 1 1 d . . . H25 H 0.7833 0.3788 0.0393 0.043 Uiso 1 1 calc R . . C26 C 0.8988(2) 0.3293(2) 0.05951(13) 0.0360(7) Uani 1 1 d . . . H26 H 0.9282 0.3260 0.0305 0.043 Uiso 1 1 calc R . . C27 C 0.9275(2) 0.3052(2) 0.10622(13) 0.0381(7) Uani 1 1 d . . . H27 H 0.9796 0.2827 0.1137 0.046 Uiso 1 1 calc R . . Ni2 Ni 0.00614(2) 0.16619(3) 0.319686(12) 0.02304(7) Uani 1 1 d . . . Ru2 Ru 0.325570(14) 0.213086(15) 0.407430(9) 0.02454(5) Uani 1 1 d . . . Cl2 Cl -0.09687(5) 0.18729(7) 0.27189(3) 0.03901(17) Uani 1 1 d . . . P3 P 0.09758(4) 0.16758(5) 0.26546(2) 0.02402(13) Uani 1 1 d . . . P4 P -0.05854(4) 0.15928(5) 0.38638(3) 0.02306(13) Uani 1 1 d . . . O3 O 0.18332(12) 0.14885(16) 0.29411(7) 0.0279(4) Uani 1 1 d . . . O4 O 0.00893(12) 0.13625(16) 0.42828(7) 0.0266(4) Uani 1 1 d . . . C28 C 0.09408(17) 0.14253(19) 0.35999(10) 0.0225(5) Uani 1 1 d . . . C29 C 0.16965(17) 0.1348(2) 0.34254(9) 0.0248(5) Uani 1 1 d . . . C30 C 0.23745(17) 0.11123(19) 0.37118(10) 0.0239(5) Uani 1 1 d . . . C31 C 0.22478(16) 0.1011(2) 0.42199(9) 0.0231(5) Uani 1 1 d . . . C32 C 0.14668(16) 0.1120(2) 0.44106(9) 0.0235(5) Uani 1 1 d . . . H32 H 0.1378 0.1070 0.4746 0.028 Uiso 1 1 calc R . . C33 C 0.08506(16) 0.12954(19) 0.41075(10) 0.0231(5) Uani 1 1 d . . . C34 C 0.31588(18) 0.0998(2) 0.35166(11) 0.0290(6) Uani 1 1 d . . . H34 H 0.3243 0.1085 0.3183 0.035 Uiso 1 1 calc R . . C35 C 0.38067(18) 0.0757(2) 0.38174(12) 0.0324(6) Uani 1 1 d . . . H35 H 0.4319 0.0647 0.3684 0.039 Uiso 1 1 calc R . . C36 C 0.36922(19) 0.0676(2) 0.43215(12) 0.0319(6) Uani 1 1 d . . . H36 H 0.4128 0.0512 0.4524 0.038 Uiso 1 1 calc R . . C37 C 0.29336(18) 0.0841(2) 0.45190(11) 0.0275(6) Uani 1 1 d . . . H37 H 0.2872 0.0840 0.4857 0.033 Uiso 1 1 calc R . . C38 C 0.1166(2) 0.2856(2) 0.23554(11) 0.0314(6) Uani 1 1 d . . . H38 H 0.0697 0.3008 0.2147 0.038 Uiso 1 1 calc R . . C39 C 0.1223(3) 0.3661(3) 0.27345(14) 0.0459(8) Uani 1 1 d . . . H39A H 0.1708 0.3565 0.2924 0.069 Uiso 1 1 calc R . . H39B H 0.0757 0.3627 0.2945 0.069 Uiso 1 1 calc R . . H39C H 0.1241 0.4308 0.2578 0.069 Uiso 1 1 calc R . . C40 C 0.1906(2) 0.2820(3) 0.20379(13) 0.0402(7) Uani 1 1 d . . . H40A H 0.2001 0.3473 0.1898 0.060 Uiso 1 1 calc R . . H40B H 0.1825 0.2338 0.1781 0.060 Uiso 1 1 calc R . . H40C H 0.2368 0.2626 0.2231 0.060 Uiso 1 1 calc R . . C41 C 0.1023(2) 0.0696(2) 0.22097(10) 0.0313(6) Uani 1 1 d . . . H41 H 0.1546 0.0748 0.2040 0.038 Uiso 1 1 calc R . . C42 C 0.0361(3) 0.0791(3) 0.18389(12) 0.0459(8) Uani 1 1 d . . . H42A H 0.0422 0.0274 0.1596 0.069 Uiso 1 1 calc R . . H42B H 0.0394 0.1439 0.1685 0.069 Uiso 1 1 calc R . . H42C H -0.0157 0.0721 0.1997 0.069 Uiso 1 1 calc R . . C43 C 0.0998(3) -0.0303(3) 0.24691(14) 0.0474(9) Uani 1 1 d . . . H43A H 0.0475 -0.0390 0.2619 0.071 Uiso 1 1 calc R . . H43B H 0.1413 -0.0321 0.2716 0.071 Uiso 1 1 calc R . . H43C H 0.1089 -0.0835 0.2238 0.071 Uiso 1 1 calc R . . C44 C -0.1065(2) 0.2695(2) 0.41035(12) 0.0386(7) Uani 1 1 d . . . H44 H -0.1228 0.2557 0.4441 0.046 Uiso 1 1 calc R . . C45 C -0.0442(3) 0.3523(3) 0.41100(17) 0.0593(12) Uani 1 1 d . . . H45A H -0.0259 0.3652 0.3783 0.089 Uiso 1 1 calc R . . H45B H 0.0011 0.3323 0.4309 0.089 Uiso 1 1 calc R . . H45C H -0.0681 0.4124 0.4243 0.089 Uiso 1 1 calc R . . C46 C -0.1809(3) 0.2972(3) 0.38184(17) 0.0556(11) Uani 1 1 d . . . H46A H -0.2052 0.3562 0.3959 0.083 Uiso 1 1 calc R . . H46B H -0.2190 0.2425 0.3828 0.083 Uiso 1 1 calc R . . H46C H -0.1661 0.3107 0.3485 0.083 Uiso 1 1 calc R . . C47 C -0.12663(18) 0.0555(2) 0.39323(11) 0.0319(6) Uani 1 1 d . . . H47 H -0.1753 0.0693 0.3737 0.038 Uiso 1 1 calc R . . C48 C -0.1525(2) 0.0406(3) 0.44521(13) 0.0519(10) Uani 1 1 d . . . H48A H -0.1870 -0.0175 0.4474 0.078 Uiso 1 1 calc R . . H48B H -0.1817 0.0990 0.4562 0.078 Uiso 1 1 calc R . . H48C H -0.1053 0.0309 0.4654 0.078 Uiso 1 1 calc R . . C49 C -0.0860(3) -0.0356(3) 0.37252(18) 0.0568(11) Uani 1 1 d . . . H49A H -0.0803 -0.0280 0.3378 0.085 Uiso 1 1 calc R . . H49B H -0.1183 -0.0941 0.3794 0.085 Uiso 1 1 calc R . . H49C H -0.0332 -0.0433 0.3871 0.085 Uiso 1 1 calc R . . C50 C 0.3248(3) 0.3422(2) 0.45426(15) 0.0452(8) Uani 1 1 d . . . H50 H 0.3066 0.3420 0.4865 0.054 Uiso 1 1 calc R . . C51 C 0.2786(2) 0.3617(2) 0.41456(17) 0.0471(9) Uani 1 1 d . . . H51 H 0.2232 0.3765 0.4150 0.057 Uiso 1 1 calc R . . C52 C 0.3263(3) 0.3562(3) 0.37347(15) 0.0537(11) Uani 1 1 d . . . H52 H 0.3094 0.3669 0.3414 0.064 Uiso 1 1 calc R . . C53 C 0.4037(3) 0.3320(3) 0.3885(2) 0.0658(15) Uani 1 1 d . . . H53 H 0.4487 0.3233 0.3683 0.079 Uiso 1 1 calc R . . C54 C 0.4028(3) 0.3228(3) 0.43942(19) 0.0526(11) Uani 1 1 d . . . H54 H 0.4467 0.3066 0.4594 0.063 Uiso 1 1 calc R . . P5 P 0.12272(5) 0.16602(7) 0.03914(3) 0.03382(17) Uani 1 1 d . . . F1 F 0.1211(3) 0.1898(3) 0.09426(10) 0.1041(14) Uani 1 1 d . . . F2 F 0.05307(17) 0.0899(2) 0.04642(15) 0.0885(11) Uani 1 1 d . . . F3 F 0.18548(17) 0.0796(2) 0.04778(10) 0.0707(8) Uani 1 1 d . . . F4 F 0.19270(18) 0.2428(3) 0.03031(12) 0.0814(10) Uani 1 1 d . . . F5 F 0.06023(17) 0.2510(2) 0.02932(10) 0.0647(7) Uani 1 1 d . . . F6 F 0.12486(18) 0.1424(2) -0.01653(8) 0.0601(7) Uani 1 1 d . . . P6 P 0.38859(5) 0.64632(7) 0.04707(3) 0.03521(17) Uani 1 1 d . . . F7 F 0.4482(2) 0.6473(4) 0.09027(13) 0.1160(17) Uani 1 1 d . . . F8 F 0.4267(4) 0.5405(3) 0.03754(17) 0.155(2) Uani 1 1 d . . . F9 F 0.4523(2) 0.6897(3) 0.01179(12) 0.0906(11) Uani 1 1 d . . . F10 F 0.3551(5) 0.7480(3) 0.05457(18) 0.184(3) Uani 1 1 d . . . F11 F 0.3259(2) 0.6049(4) 0.08422(15) 0.1249(18) Uani 1 1 d . . . F12 F 0.3346(2) 0.6315(4) 0.00290(14) 0.1230(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02406(16) 0.02857(17) 0.02548(16) 0.00336(13) 0.00235(13) 0.00156(14) Ru1 0.02368(9) 0.01880(9) 0.02921(10) -0.00093(7) 0.00249(9) -0.00196(8) Cl1 0.0329(4) 0.0563(5) 0.0367(4) 0.0047(3) 0.0111(3) 0.0046(4) P1 0.0229(3) 0.0273(3) 0.0299(3) 0.0032(3) -0.0010(3) 0.0007(3) P2 0.0269(3) 0.0285(3) 0.0250(3) 0.0010(3) 0.0004(3) 0.0028(3) O1 0.0245(10) 0.0433(12) 0.0269(9) 0.0041(8) -0.0015(8) 0.0008(9) O2 0.0255(9) 0.0340(10) 0.0260(9) 0.0008(8) -0.0012(7) 0.0040(8) C1 0.0228(12) 0.0248(12) 0.0281(13) 0.0008(10) 0.0001(10) 0.0011(10) C2 0.0236(12) 0.0256(12) 0.0251(12) 0.0016(10) -0.0004(10) -0.0003(10) C3 0.0260(13) 0.0303(13) 0.0267(12) 0.0013(10) -0.0021(10) -0.0025(11) C4 0.0289(13) 0.0209(12) 0.0288(13) -0.0032(10) 0.0010(10) -0.0014(11) C5 0.0237(12) 0.0178(11) 0.0314(13) -0.0019(10) 0.0012(10) 0.0009(10) C6 0.0268(13) 0.0210(11) 0.0257(12) 0.0019(9) -0.0034(10) 0.0001(10) C7 0.0298(14) 0.0300(14) 0.0306(14) -0.0063(11) 0.0028(11) -0.0038(12) C8 0.0305(14) 0.0279(13) 0.0340(14) -0.0094(11) 0.0056(11) -0.0008(11) C9 0.0262(12) 0.0225(12) 0.0427(16) -0.0013(11) 0.0048(12) 0.0031(10) C10 0.0264(12) 0.0172(10) 0.0334(13) 0.0009(9) -0.0025(11) -0.0003(10) C11 0.0320(14) 0.0264(13) 0.0371(15) 0.0025(11) -0.0040(12) 0.0011(12) C12 0.0446(18) 0.0315(15) 0.0506(19) 0.0046(14) -0.0095(16) -0.0071(15) C13 0.065(3) 0.0374(18) 0.060(2) 0.0043(16) -0.032(2) 0.0094(19) C14 0.0289(14) 0.0306(14) 0.0413(16) -0.0001(12) -0.0041(12) -0.0023(12) C15 0.057(2) 0.0345(18) 0.081(3) -0.0085(19) 0.017(2) -0.0010(18) C16 0.0352(18) 0.052(2) 0.066(2) -0.0150(19) 0.0103(17) -0.0125(17) C17 0.0369(16) 0.0372(15) 0.0356(15) -0.0064(12) -0.0001(13) -0.0019(14) C18 0.079(3) 0.0342(17) 0.057(2) -0.0010(16) 0.006(2) -0.018(2) C19 0.067(3) 0.046(2) 0.0428(19) -0.0111(16) 0.0104(18) 0.007(2) C20 0.0373(16) 0.0325(14) 0.0272(13) 0.0045(11) 0.0035(12) 0.0032(13) C21 0.093(3) 0.0347(19) 0.042(2) 0.0041(15) -0.003(2) -0.014(2) C22 0.049(2) 0.057(2) 0.0431(19) 0.0131(17) -0.0044(16) 0.0156(19) C23 0.068(3) 0.0235(14) 0.0395(17) -0.0058(12) 0.0018(17) -0.0128(16) C24 0.0488(19) 0.0170(12) 0.058(2) -0.0048(13) 0.0153(17) -0.0023(13) C25 0.0387(17) 0.0220(12) 0.0464(17) 0.0071(12) 0.0051(14) -0.0031(12) C26 0.0343(16) 0.0271(14) 0.0465(18) 0.0039(13) 0.0039(14) -0.0084(13) C27 0.0363(16) 0.0259(14) 0.0522(19) 0.0028(13) -0.0096(14) -0.0105(13) Ni2 0.02207(15) 0.02576(16) 0.02129(15) 0.00211(12) -0.00118(12) 0.00058(13) Ru2 0.02182(9) 0.01963(9) 0.03217(11) 0.00260(8) 0.00042(10) -0.00117(8) Cl2 0.0308(4) 0.0514(5) 0.0348(4) 0.0036(3) -0.0086(3) 0.0051(3) P3 0.0258(3) 0.0251(3) 0.0213(3) 0.0011(2) 0.0000(3) -0.0003(3) P4 0.0220(3) 0.0231(3) 0.0241(3) 0.0017(2) 0.0013(2) 0.0022(3) O3 0.0244(9) 0.0370(11) 0.0223(9) 0.0011(7) 0.0024(7) 0.0020(8) O4 0.0221(9) 0.0340(10) 0.0236(8) 0.0020(7) -0.0003(7) -0.0009(8) C28 0.0225(12) 0.0210(11) 0.0240(11) 0.0007(9) -0.0010(9) 0.0019(10) C29 0.0255(12) 0.0253(11) 0.0235(11) -0.0010(9) -0.0013(10) -0.0008(11) C30 0.0239(12) 0.0192(11) 0.0287(13) 0.0006(9) -0.0009(10) -0.0017(10) C31 0.0236(12) 0.0186(11) 0.0272(12) 0.0011(9) -0.0048(9) -0.0033(10) C32 0.0248(12) 0.0231(11) 0.0227(11) 0.0046(9) -0.0022(9) -0.0038(10) C33 0.0226(11) 0.0224(11) 0.0244(11) 0.0014(10) 0.0004(10) -0.0008(9) C34 0.0258(13) 0.0254(12) 0.0357(14) -0.0016(10) 0.0009(11) 0.0032(11) C35 0.0254(13) 0.0248(13) 0.0470(17) -0.0039(12) -0.0028(12) 0.0047(11) C36 0.0289(14) 0.0231(13) 0.0438(16) 0.0046(12) -0.0089(12) 0.0023(11) C37 0.0299(13) 0.0204(12) 0.0321(14) 0.0058(10) -0.0065(11) -0.0041(10) C38 0.0348(15) 0.0267(13) 0.0329(14) 0.0061(11) 0.0019(12) 0.0003(12) C39 0.055(2) 0.0292(15) 0.054(2) -0.0060(14) 0.0086(18) -0.0062(16) C40 0.0437(19) 0.0358(16) 0.0412(17) 0.0063(13) 0.0106(14) -0.0037(14) C41 0.0380(16) 0.0275(13) 0.0285(13) -0.0021(11) -0.0003(11) 0.0013(12) C42 0.063(2) 0.0437(18) 0.0312(15) -0.0062(14) -0.0124(16) 0.0007(18) C43 0.064(2) 0.0261(15) 0.052(2) -0.0019(14) -0.0033(18) 0.0026(17) C44 0.0529(19) 0.0301(14) 0.0328(14) -0.0010(12) 0.0073(15) 0.0135(14) C45 0.090(4) 0.0258(15) 0.062(2) -0.0085(17) -0.018(3) 0.0037(19) C46 0.051(2) 0.051(2) 0.065(2) 0.0091(18) 0.007(2) 0.031(2) C47 0.0262(13) 0.0338(15) 0.0358(15) 0.0084(12) -0.0049(11) -0.0051(12) C48 0.044(2) 0.068(3) 0.0443(19) 0.0164(18) 0.0038(16) -0.0218(19) C49 0.059(3) 0.0304(17) 0.080(3) -0.0060(18) 0.004(2) -0.0086(18) C50 0.062(2) 0.0228(13) 0.051(2) -0.0056(13) 0.0023(19) -0.0065(16) C51 0.0413(18) 0.0180(13) 0.082(3) 0.0061(15) 0.0065(19) 0.0031(13) C52 0.089(3) 0.0265(15) 0.0452(19) 0.0135(13) -0.002(2) -0.016(2) C53 0.061(3) 0.0305(18) 0.106(4) -0.015(2) 0.049(3) -0.0237(19) C54 0.042(2) 0.0268(16) 0.088(3) -0.0095(18) -0.017(2) -0.0071(16) P5 0.0301(4) 0.0363(4) 0.0350(4) 0.0028(3) 0.0012(3) -0.0010(3) F1 0.157(4) 0.122(3) 0.0333(13) -0.0084(16) 0.0013(19) 0.031(3) F2 0.0458(15) 0.0666(19) 0.153(3) 0.043(2) 0.0129(18) -0.0189(14) F3 0.0638(17) 0.0781(19) 0.0704(17) 0.0152(14) -0.0033(14) 0.0360(15) F4 0.0601(17) 0.090(2) 0.094(2) 0.0124(18) -0.0168(16) -0.0417(17) F5 0.0698(17) 0.0523(14) 0.0719(16) 0.0144(12) 0.0237(14) 0.0308(14) F6 0.0732(18) 0.0648(16) 0.0423(12) -0.0105(11) -0.0050(12) 0.0146(14) P6 0.0326(4) 0.0360(4) 0.0370(4) 0.0050(3) -0.0057(3) -0.0055(3) F7 0.0600(19) 0.226(5) 0.0617(19) 0.017(3) -0.0163(16) -0.002(3) F8 0.282(8) 0.079(3) 0.104(3) 0.020(2) 0.028(4) 0.069(4) F9 0.073(2) 0.130(3) 0.0682(19) 0.0258(19) 0.0184(16) -0.024(2) F10 0.351(9) 0.061(2) 0.139(4) 0.025(2) 0.128(5) 0.091(4) F11 0.061(2) 0.193(5) 0.121(3) 0.089(3) 0.010(2) -0.033(3) F12 0.075(2) 0.207(5) 0.087(2) -0.018(3) -0.038(2) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.871(3) . ? Ni1 P2 2.1593(9) . ? Ni1 P1 2.1667(8) . ? Ni1 Cl1 2.1903(9) . ? Ru1 C27 2.153(3) . ? Ru1 C23 2.164(3) . ? Ru1 C26 2.174(3) . ? Ru1 C24 2.181(3) . ? Ru1 C25 2.181(3) . ? Ru1 C10 2.184(3) . ? Ru1 C9 2.197(3) . ? Ru1 C8 2.208(3) . ? Ru1 C7 2.218(3) . ? Ru1 C5 2.264(3) . ? Ru1 C4 2.317(3) . ? P1 O1 1.650(2) . ? P1 C11 1.825(3) . ? P1 C14 1.827(3) . ? P2 O2 1.672(2) . ? P2 C20 1.821(3) . ? P2 C17 1.823(3) . ? O1 C2 1.369(3) . ? O2 C6 1.378(3) . ? C1 C6 1.365(4) . ? C1 C2 1.444(4) . ? C2 C3 1.364(4) . ? C3 C4 1.425(4) . ? C3 H3 0.9500 . ? C4 C7 1.428(4) . ? C4 C5 1.449(4) . ? C5 C10 1.430(4) . ? C5 C6 1.433(4) . ? C7 C8 1.412(4) . ? C7 H7 0.9500 . ? C8 C9 1.410(4) . ? C8 H8 0.9500 . ? C9 C10 1.406(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C13 1.523(5) . ? C11 C12 1.532(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.514(5) . ? C14 C15 1.527(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.526(5) . ? C17 C18 1.528(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.528(5) . ? C20 C22 1.533(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.411(6) . ? C23 C27 1.417(6) . ? C23 H23 0.9500 . ? C24 C25 1.417(5) . ? C24 H24 0.9500 . ? C25 C26 1.425(5) . ? C25 H25 0.9500 . ? C26 C27 1.427(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? Ni2 C28 1.883(3) . ? Ni2 P3 2.1570(8) . ? Ni2 P4 2.1585(8) . ? Ni2 Cl2 2.2023(8) . ? Ru2 C53 2.146(4) . ? Ru2 C52 2.160(3) . ? Ru2 C54 2.166(4) . ? Ru2 C51 2.173(3) . ? Ru2 C50 2.185(3) . ? Ru2 C34 2.193(3) . ? Ru2 C35 2.201(3) . ? Ru2 C37 2.212(3) . ? Ru2 C36 2.214(3) . ? Ru2 C30 2.262(3) . ? Ru2 C31 2.310(3) . ? P3 O3 1.666(2) . ? P3 C41 1.821(3) . ? P3 C38 1.833(3) . ? P4 O4 1.658(2) . ? P4 C47 1.823(3) . ? P4 C44 1.825(3) . ? O3 C29 1.385(3) . ? O4 C33 1.372(3) . ? C28 C29 1.363(4) . ? C28 C33 1.436(4) . ? C29 C30 1.427(4) . ? C30 C34 1.434(4) . ? C30 C31 1.442(4) . ? C31 C32 1.423(4) . ? C31 C37 1.440(4) . ? C32 C33 1.357(4) . ? C32 H32 0.9500 . ? C34 C35 1.412(4) . ? C34 H34 0.9500 . ? C35 C36 1.425(5) . ? C35 H35 0.9500 . ? C36 C37 1.406(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.523(5) . ? C38 C40 1.528(5) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.524(5) . ? C41 C43 1.537(5) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.527(5) . ? C44 C45 1.534(6) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.525(5) . ? C47 C48 1.529(5) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.379(6) . ? C50 C54 1.399(6) . ? C50 H50 0.9500 . ? C51 C52 1.402(6) . ? C51 H51 0.9500 . ? C52 C53 1.404(8) . ? C52 H52 0.9500 . ? C53 C54 1.429(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? P5 F1 1.573(3) . ? P5 F2 1.573(3) . ? P5 F5 1.582(3) . ? P5 F6 1.588(2) . ? P5 F4 1.589(3) . ? P5 F3 1.594(3) . ? P6 F10 1.503(4) . ? P6 F12 1.543(3) . ? P6 F7 1.567(3) . ? P6 F9 1.569(3) . ? P6 F11 1.581(3) . ? P6 F8 1.593(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 P2 82.44(9) . . ? C1 Ni1 P1 82.58(9) . . ? P2 Ni1 P1 164.43(3) . . ? C1 Ni1 Cl1 178.06(9) . . ? P2 Ni1 Cl1 96.28(3) . . ? P1 Ni1 Cl1 98.80(3) . . ? C27 Ru1 C23 38.31(15) . . ? C27 Ru1 C26 38.52(13) . . ? C23 Ru1 C26 64.27(14) . . ? C27 Ru1 C24 63.60(15) . . ? C23 Ru1 C24 37.89(16) . . ? C26 Ru1 C24 63.73(13) . . ? C27 Ru1 C25 63.96(13) . . ? C23 Ru1 C25 63.83(14) . . ? C26 Ru1 C25 38.20(13) . . ? C24 Ru1 C25 37.93(13) . . ? C27 Ru1 C10 116.57(12) . . ? C23 Ru1 C10 105.08(12) . . ? C26 Ru1 C10 151.47(12) . . ? C24 Ru1 C10 125.20(12) . . ? C25 Ru1 C10 162.61(12) . . ? C27 Ru1 C9 105.42(13) . . ? C23 Ru1 C9 119.92(14) . . ? C26 Ru1 C9 122.45(12) . . ? C24 Ru1 C9 155.58(14) . . ? C25 Ru1 C9 159.29(12) . . ? C10 Ru1 C9 37.44(11) . . ? C27 Ru1 C8 115.83(13) . . ? C23 Ru1 C8 149.03(15) . . ? C26 Ru1 C8 106.81(13) . . ? C24 Ru1 C8 166.47(13) . . ? C25 Ru1 C8 128.71(13) . . ? C10 Ru1 C8 67.86(11) . . ? C9 Ru1 C8 37.33(12) . . ? C27 Ru1 C7 143.60(13) . . ? C23 Ru1 C7 173.11(14) . . ? C26 Ru1 C7 113.50(13) . . ? C24 Ru1 C7 135.27(14) . . ? C25 Ru1 C7 110.16(13) . . ? C10 Ru1 C7 79.89(11) . . ? C9 Ru1 C7 66.92(12) . . ? C8 Ru1 C7 37.19(11) . . ? C27 Ru1 C5 145.57(12) . . ? C23 Ru1 C5 114.30(12) . . ? C26 Ru1 C5 170.50(12) . . ? C24 Ru1 C5 108.97(12) . . ? C25 Ru1 C5 132.31(12) . . ? C10 Ru1 C5 37.46(10) . . ? C9 Ru1 C5 66.79(10) . . ? C8 Ru1 C5 79.21(11) . . ? C7 Ru1 C5 66.71(11) . . ? C27 Ru1 C4 176.10(12) . . ? C23 Ru1 C4 140.75(14) . . ? C26 Ru1 C4 138.40(12) . . ? C24 Ru1 C4 113.43(13) . . ? C25 Ru1 C4 112.14(12) . . ? C10 Ru1 C4 67.08(10) . . ? C9 Ru1 C4 78.31(11) . . ? C8 Ru1 C4 66.39(11) . . ? C7 Ru1 C4 36.62(10) . . ? C5 Ru1 C4 36.85(10) . . ? O1 P1 C11 102.57(14) . . ? O1 P1 C14 100.71(14) . . ? C11 P1 C14 109.16(15) . . ? O1 P1 Ni1 105.88(8) . . ? C11 P1 Ni1 113.85(11) . . ? C14 P1 Ni1 121.88(11) . . ? O2 P2 C20 102.54(13) . . ? O2 P2 C17 101.42(14) . . ? C20 P2 C17 107.03(15) . . ? O2 P2 Ni1 105.24(8) . . ? C20 P2 Ni1 117.55(11) . . ? C17 P2 Ni1 120.22(12) . . ? C2 O1 P1 113.11(18) . . ? C6 O2 P2 109.76(18) . . ? C6 C1 C2 117.0(3) . . ? C6 C1 Ni1 121.3(2) . . ? C2 C1 Ni1 121.7(2) . . ? C3 C2 O1 119.8(3) . . ? C3 C2 C1 123.6(3) . . ? O1 C2 C1 116.6(2) . . ? C2 C3 C4 118.5(3) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C7 121.6(3) . . ? C3 C4 C5 120.4(3) . . ? C7 C4 C5 117.9(3) . . ? C3 C4 Ru1 132.1(2) . . ? C7 C4 Ru1 67.95(16) . . ? C5 C4 Ru1 69.61(16) . . ? C10 C5 C6 123.3(3) . . ? C10 C5 C4 119.7(3) . . ? C6 C5 C4 117.0(2) . . ? C10 C5 Ru1 68.21(15) . . ? C6 C5 Ru1 128.66(19) . . ? C4 C5 Ru1 73.54(16) . . ? C1 C6 O2 120.2(3) . . ? C1 C6 C5 123.3(2) . . ? O2 C6 C5 116.4(2) . . ? C8 C7 C4 121.6(3) . . ? C8 C7 Ru1 71.02(17) . . ? C4 C7 Ru1 75.43(17) . . ? C8 C7 H7 119.2 . . ? C4 C7 H7 119.2 . . ? Ru1 C7 H7 126.3 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 Ru1 70.91(16) . . ? C7 C8 Ru1 71.79(17) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? Ru1 C8 H8 129.2 . . ? C10 C9 C8 121.1(3) . . ? C10 C9 Ru1 70.75(15) . . ? C8 C9 Ru1 71.75(17) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? Ru1 C9 H9 130.8 . . ? C9 C10 C5 120.0(3) . . ? C9 C10 Ru1 71.82(16) . . ? C5 C10 Ru1 74.33(15) . . ? C9 C10 H10 120.0 . . ? C5 C10 H10 120.0 . . ? Ru1 C10 H10 125.6 . . ? C13 C11 C12 110.6(3) . . ? C13 C11 P1 114.2(2) . . ? C12 C11 P1 108.4(2) . . ? C13 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? P1 C11 H11 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 111.6(3) . . ? C16 C14 P1 111.2(2) . . ? C15 C14 P1 108.6(3) . . ? C16 C14 H14 108.4 . . ? C15 C14 H14 108.4 . . ? P1 C14 H14 108.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 111.2(3) . . ? C19 C17 P2 111.1(3) . . ? C18 C17 P2 110.0(2) . . ? C19 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? P2 C17 H17 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 112.3(3) . . ? C21 C20 P2 108.5(2) . . ? C22 C20 P2 113.1(2) . . ? C21 C20 H20 107.6 . . ? C22 C20 H20 107.6 . . ? P2 C20 H20 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C27 107.7(3) . . ? C24 C23 Ru1 71.7(2) . . ? C27 C23 Ru1 70.39(18) . . ? C24 C23 H23 126.1 . . ? C27 C23 H23 126.1 . . ? Ru1 C23 H23 123.4 . . ? C23 C24 C25 108.6(3) . . ? C23 C24 Ru1 70.43(19) . . ? C25 C24 Ru1 71.04(18) . . ? C23 C24 H24 125.7 . . ? C25 C24 H24 125.7 . . ? Ru1 C24 H24 124.4 . . ? C24 C25 C26 108.0(3) . . ? C24 C25 Ru1 71.04(18) . . ? C26 C25 Ru1 70.66(18) . . ? C24 C25 H25 126.0 . . ? C26 C25 H25 126.0 . . ? Ru1 C25 H25 123.9 . . ? C25 C26 C27 107.2(3) . . ? C25 C26 Ru1 71.14(18) . . ? C27 C26 Ru1 69.92(18) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? Ru1 C26 H26 124.2 . . ? C23 C27 C26 108.5(3) . . ? C23 C27 Ru1 71.3(2) . . ? C26 C27 Ru1 71.57(18) . . ? C23 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? Ru1 C27 H27 123.0 . . ? C28 Ni2 P3 82.14(9) . . ? C28 Ni2 P4 82.61(9) . . ? P3 Ni2 P4 164.74(3) . . ? C28 Ni2 Cl2 177.64(9) . . ? P3 Ni2 Cl2 97.60(3) . . ? P4 Ni2 Cl2 97.66(3) . . ? C53 Ru2 C52 38.1(2) . . ? C53 Ru2 C54 38.71(19) . . ? C52 Ru2 C54 63.93(17) . . ? C53 Ru2 C51 63.13(16) . . ? C52 Ru2 C51 37.76(17) . . ? C54 Ru2 C51 62.79(16) . . ? C53 Ru2 C50 63.24(16) . . ? C52 Ru2 C50 62.81(15) . . ? C54 Ru2 C50 37.51(17) . . ? C51 Ru2 C50 36.88(16) . . ? C53 Ru2 C34 113.32(15) . . ? C52 Ru2 C34 108.53(14) . . ? C54 Ru2 C34 144.88(16) . . ? C51 Ru2 C34 133.44(15) . . ? C50 Ru2 C34 170.23(14) . . ? C53 Ru2 C35 107.37(15) . . ? C52 Ru2 C35 127.95(16) . . ? C54 Ru2 C35 117.67(14) . . ? C51 Ru2 C35 165.38(15) . . ? C50 Ru2 C35 151.17(15) . . ? C34 Ru2 C35 37.49(11) . . ? C53 Ru2 C37 151.95(19) . . ? C52 Ru2 C37 163.37(17) . . ? C54 Ru2 C37 117.25(15) . . ? C51 Ru2 C37 126.34(14) . . ? C50 Ru2 C37 107.20(13) . . ? C34 Ru2 C37 80.04(11) . . ? C35 Ru2 C37 67.46(12) . . ? C53 Ru2 C36 122.96(18) . . ? C52 Ru2 C36 159.26(18) . . ? C54 Ru2 C36 106.57(14) . . ? C51 Ru2 C36 156.55(15) . . ? C50 Ru2 C36 121.94(14) . . ? C34 Ru2 C36 67.80(12) . . ? C35 Ru2 C36 37.67(12) . . ? C37 Ru2 C36 37.04(12) . . ? C53 Ru2 C30 138.41(18) . . ? C52 Ru2 C30 110.84(15) . . ? C54 Ru2 C30 174.24(14) . . ? C51 Ru2 C30 111.69(13) . . ? C50 Ru2 C30 138.82(14) . . ? C34 Ru2 C30 37.50(10) . . ? C35 Ru2 C30 67.18(11) . . ? C37 Ru2 C30 66.96(10) . . ? C36 Ru2 C30 79.17(11) . . ? C53 Ru2 C31 170.32(18) . . ? C52 Ru2 C31 132.25(16) . . ? C54 Ru2 C31 144.82(16) . . ? C51 Ru2 C31 109.11(12) . . ? C50 Ru2 C31 114.62(13) . . ? C34 Ru2 C31 67.09(11) . . ? C35 Ru2 C31 78.98(11) . . ? C37 Ru2 C31 37.06(10) . . ? C36 Ru2 C31 66.53(11) . . ? C30 Ru2 C31 36.74(10) . . ? O3 P3 C41 100.28(13) . . ? O3 P3 C38 101.62(13) . . ? C41 P3 C38 108.54(14) . . ? O3 P3 Ni2 106.06(7) . . ? C41 P3 Ni2 120.27(11) . . ? C38 P3 Ni2 116.86(11) . . ? O4 P4 C47 102.04(12) . . ? O4 P4 C44 101.35(14) . . ? C47 P4 C44 108.47(17) . . ? O4 P4 Ni2 105.87(8) . . ? C47 P4 Ni2 116.09(11) . . ? C44 P4 Ni2 120.21(12) . . ? C29 O3 P3 110.25(18) . . ? C33 O4 P4 113.37(17) . . ? C29 C28 C33 116.2(2) . . ? C29 C28 Ni2 121.9(2) . . ? C33 C28 Ni2 121.8(2) . . ? C28 C29 O3 119.6(2) . . ? C28 C29 C30 124.0(2) . . ? O3 C29 C30 116.4(2) . . ? C29 C30 C34 122.9(3) . . ? C29 C30 C31 117.1(2) . . ? C34 C30 C31 120.0(3) . . ? C29 C30 Ru2 129.41(19) . . ? C34 C30 Ru2 68.64(16) . . ? C31 C30 Ru2 73.43(16) . . ? C32 C31 C37 122.4(2) . . ? C32 C31 C30 119.7(2) . . ? C37 C31 C30 117.9(3) . . ? C32 C31 Ru2 132.27(19) . . ? C37 C31 Ru2 67.78(15) . . ? C30 C31 Ru2 69.83(15) . . ? C33 C32 C31 119.1(2) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 O4 119.9(2) . . ? C32 C33 C28 123.8(3) . . ? O4 C33 C28 116.3(2) . . ? C35 C34 C30 120.4(3) . . ? C35 C34 Ru2 71.54(17) . . ? C30 C34 Ru2 73.86(16) . . ? C35 C34 H34 119.8 . . ? C30 C34 H34 119.8 . . ? Ru2 C34 H34 126.7 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 Ru2 70.97(17) . . ? C36 C35 Ru2 71.67(18) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? Ru2 C35 H35 129.9 . . ? C37 C36 C35 119.9(3) . . ? C37 C36 Ru2 71.42(17) . . ? C35 C36 Ru2 70.66(17) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? Ru2 C36 H36 130.4 . . ? C36 C37 C31 121.5(3) . . ? C36 C37 Ru2 71.54(17) . . ? C31 C37 Ru2 75.16(15) . . ? C36 C37 H37 119.3 . . ? C31 C37 H37 119.3 . . ? Ru2 C37 H37 125.9 . . ? C39 C38 C40 112.0(3) . . ? C39 C38 P3 108.6(2) . . ? C40 C38 P3 112.2(2) . . ? C39 C38 H38 107.9 . . ? C40 C38 H38 107.9 . . ? P3 C38 H38 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 112.0(3) . . ? C42 C41 P3 111.7(2) . . ? C43 C41 P3 108.7(2) . . ? C42 C41 H41 108.1 . . ? C43 C41 H41 108.1 . . ? P3 C41 H41 108.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C45 112.5(3) . . ? C46 C44 P4 111.8(3) . . ? C45 C44 P4 107.6(3) . . ? C46 C44 H44 108.3 . . ? C45 C44 H44 108.3 . . ? P4 C44 H44 108.3 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C48 112.4(3) . . ? C49 C47 P4 107.7(2) . . ? C48 C47 P4 112.3(2) . . ? C49 C47 H47 108.1 . . ? C48 C47 H47 108.1 . . ? P4 C47 H47 108.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C54 108.9(4) . . ? C51 C50 Ru2 71.1(2) . . ? C54 C50 Ru2 70.5(2) . . ? C51 C50 H50 125.5 . . ? C54 C50 H50 125.5 . . ? Ru2 C50 H50 124.5 . . ? C50 C51 C52 109.0(4) . . ? C50 C51 Ru2 72.0(2) . . ? C52 C51 Ru2 70.6(2) . . ? C50 C51 H51 125.5 . . ? C52 C51 H51 125.5 . . ? Ru2 C51 H51 123.5 . . ? C51 C52 C53 107.3(4) . . ? C51 C52 Ru2 71.63(19) . . ? C53 C52 Ru2 70.4(2) . . ? C51 C52 H52 126.3 . . ? C53 C52 H52 126.3 . . ? Ru2 C52 H52 123.3 . . ? C52 C53 C54 107.9(4) . . ? C52 C53 Ru2 71.5(2) . . ? C54 C53 Ru2 71.4(2) . . ? C52 C53 H53 126.1 . . ? C54 C53 H53 126.1 . . ? Ru2 C53 H53 122.7 . . ? C50 C54 C53 106.8(4) . . ? C50 C54 Ru2 72.0(2) . . ? C53 C54 Ru2 69.9(2) . . ? C50 C54 H54 126.6 . . ? C53 C54 H54 126.6 . . ? Ru2 C54 H54 123.2 . . ? F1 P5 F2 89.7(2) . . ? F1 P5 F5 90.47(19) . . ? F2 P5 F5 90.44(17) . . ? F1 P5 F6 179.6(2) . . ? F2 P5 F6 90.6(2) . . ? F5 P5 F6 89.58(15) . . ? F1 P5 F4 91.8(2) . . ? F2 P5 F4 178.5(2) . . ? F5 P5 F4 89.20(18) . . ? F6 P5 F4 87.89(18) . . ? F1 P5 F3 90.84(19) . . ? F2 P5 F3 89.39(17) . . ? F5 P5 F3 178.67(17) . . ? F6 P5 F3 89.11(15) . . ? F4 P5 F3 90.94(19) . . ? F10 P6 F12 90.7(3) . . ? F10 P6 F7 97.1(3) . . ? F12 P6 F7 172.2(3) . . ? F10 P6 F9 90.0(3) . . ? F12 P6 F9 87.0(2) . . ? F7 P6 F9 92.6(2) . . ? F10 P6 F11 89.1(3) . . ? F12 P6 F11 95.0(2) . . ? F7 P6 F11 85.6(2) . . ? F9 P6 F11 177.8(3) . . ? F10 P6 F8 177.5(3) . . ? F12 P6 F8 89.2(3) . . ? F7 P6 F8 83.1(3) . . ? F9 P6 F8 87.6(3) . . ? F11 P6 F8 93.3(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.742 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.083 #============================================================================== data_compound-4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl O2 P2 Pd Ru, F6 P' _chemical_formula_sum 'C27 H38 Cl F6 O2 P3 Pd Ru' _chemical_formula_weight 844.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9395(11) _cell_length_b 13.5596(9) _cell_length_c 28.602(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6569.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8209 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.82 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.7437 _exptl_absorpt_correction_T_max 0.9186 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector 01-67' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 51765 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.37 _reflns_number_total 6034 _reflns_number_gt 3703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _solved_by 'Simon Hernandez-Ortega' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6034 _refine_ls_number_parameters 467 _refine_ls_number_restraints 579 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2271 _refine_ls_wR_factor_gt 0.2031 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.32873(5) 0.70418(7) 0.09536(4) 0.0535(3) Uani 1 1 d . . . Pd Pd 0.01274(5) 0.65272(7) 0.18338(3) 0.0524(3) Uani 1 1 d . . . Cl Cl -0.0939(2) 0.6744(4) 0.23589(14) 0.1029(14) Uani 1 1 d . . . P1 P 0.1125(2) 0.6500(3) 0.23645(11) 0.0640(9) Uani 1 1 d . A . P2 P -0.05258(18) 0.6558(2) 0.11352(11) 0.0562(8) Uani 1 1 d . B . O1 O 0.1913(5) 0.6253(8) 0.2048(3) 0.083(3) Uani 1 1 d . . . O2 O 0.0172(5) 0.6332(7) 0.0745(3) 0.072(3) Uani 1 1 d . . . C1 C 0.1767(7) 0.6174(8) 0.1564(4) 0.053(3) Uani 1 1 d . . . C2 C 0.1022(6) 0.6297(8) 0.1419(3) 0.044(3) Uani 1 1 d . . . C3 C 0.0918(6) 0.6255(8) 0.0903(4) 0.047(3) Uani 1 1 d . . . C4 C 0.1505(7) 0.6109(9) 0.0607(4) 0.059(3) Uani 1 1 d . . . H4 H 0.1418 0.6110 0.0286 0.071 Uiso 1 1 calc R . . C5 C 0.2973(7) 0.5814(9) 0.0502(5) 0.067(4) Uani 1 1 d . . . H5 H 0.2905 0.5857 0.0180 0.080 Uiso 1 1 calc R . . C6 C 0.3722(8) 0.5624(10) 0.0670(6) 0.076(2) Uani 1 1 d . . . H6 H 0.4143 0.5481 0.0472 0.092 Uiso 1 1 calc R . . C7 C 0.3803(8) 0.5659(10) 0.1133(5) 0.076(2) Uani 1 1 d . . . H7 H 0.4306 0.5553 0.1254 0.092 Uiso 1 1 calc R . . C8 C 0.3215(7) 0.5836(9) 0.1446(5) 0.076(2) Uani 1 1 d . . . H8 H 0.3323 0.5870 0.1764 0.092 Uiso 1 1 calc R . . C9 C 0.2436(6) 0.5968(8) 0.1279(4) 0.055(3) Uani 1 1 d . . . C10 C 0.2290(6) 0.5948(7) 0.0794(4) 0.047(3) Uani 1 1 d . . . C11 C 0.3148(9) 0.8437(9) 0.0588(7) 0.102(4) Uani 1 1 d . . . H11 H 0.2873 0.8525 0.0309 0.122 Uiso 1 1 calc R . . C12 C 0.3951(9) 0.8204(9) 0.0640(8) 0.104(6) Uani 1 1 d . . . H12 H 0.4299 0.8085 0.0395 0.125 Uiso 1 1 calc R . . C13 C 0.4159(14) 0.8175(13) 0.1127(8) 0.123(5) Uani 1 1 d . . . H13 H 0.4654 0.8063 0.1257 0.147 Uiso 1 1 calc R . . C14 C 0.3442(13) 0.8354(12) 0.1361(8) 0.123(5) Uani 1 1 d . . . H14 H 0.3378 0.8365 0.1683 0.147 Uiso 1 1 calc R . . C15 C 0.2850(10) 0.8511(9) 0.1041(7) 0.102(4) Uani 1 1 d . . . H15 H 0.2327 0.8647 0.1115 0.122 Uiso 1 1 calc R . . C16 C 0.1186(8) 0.5545(12) 0.2806(5) 0.094(4) Uani 1 1 d DU . . H16 H 0.0811 0.5736 0.3051 0.113 Uiso 0.544(18) 1 calc PR A 1 H16A H 0.1678 0.5643 0.2981 0.113 Uiso 0.456(18) 1 calc PR A 2 C17 C 0.1964(13) 0.536(2) 0.3055(8) 0.107(8) Uani 0.544(18) 1 d PDU A 1 H17A H 0.2149 0.5960 0.3193 0.160 Uiso 0.544(18) 1 calc PR A 1 H17B H 0.2347 0.5121 0.2835 0.160 Uiso 0.544(18) 1 calc PR A 1 H17C H 0.1888 0.4873 0.3296 0.160 Uiso 0.544(18) 1 calc PR A 1 C18 C 0.087(2) 0.4594(17) 0.2599(14) 0.107(7) Uani 0.544(18) 1 d PDU A 1 H18A H 0.0365 0.4720 0.2453 0.161 Uiso 0.544(18) 1 calc PR A 1 H18B H 0.0800 0.4114 0.2843 0.161 Uiso 0.544(18) 1 calc PR A 1 H18C H 0.1230 0.4346 0.2370 0.161 Uiso 0.544(18) 1 calc PR A 1 C17A C 0.122(2) 0.453(2) 0.2583(16) 0.106(8) Uani 0.456(18) 1 d PDU A 2 H17D H 0.1665 0.4496 0.2377 0.160 Uiso 0.456(18) 1 calc PR A 2 H17E H 0.0743 0.4419 0.2408 0.160 Uiso 0.456(18) 1 calc PR A 2 H17F H 0.1268 0.4039 0.2822 0.160 Uiso 0.456(18) 1 calc PR A 2 C18A C 0.0508(17) 0.562(3) 0.3149(10) 0.107(8) Uani 0.456(18) 1 d PDU A 2 H18D H 0.0491 0.6275 0.3277 0.161 Uiso 0.456(18) 1 calc PR A 2 H18E H 0.0581 0.5153 0.3396 0.161 Uiso 0.456(18) 1 calc PR A 2 H18F H 0.0020 0.5486 0.2990 0.161 Uiso 0.456(18) 1 calc PR A 2 C19 C 0.1377(10) 0.7687(12) 0.2625(5) 0.104(5) Uani 1 1 d DU . . H19 H 0.1880 0.7561 0.2783 0.125 Uiso 0.60(2) 1 calc PR A 1 H19A H 0.0929 0.7750 0.2839 0.125 Uiso 0.40(2) 1 calc PR A 2 C20 C 0.0842(16) 0.791(2) 0.3001(9) 0.121(8) Uani 0.60(2) 1 d PDU A 1 H20A H 0.0781 0.7340 0.3196 0.181 Uiso 0.60(2) 1 calc PR A 1 H20B H 0.0339 0.8096 0.2875 0.181 Uiso 0.60(2) 1 calc PR A 1 H20C H 0.1051 0.8446 0.3183 0.181 Uiso 0.60(2) 1 calc PR A 1 C21 C 0.158(2) 0.8388(17) 0.2261(9) 0.117(7) Uani 0.60(2) 1 d PDU A 1 H21A H 0.1955 0.8093 0.2051 0.176 Uiso 0.60(2) 1 calc PR A 1 H21B H 0.1810 0.8965 0.2401 0.176 Uiso 0.60(2) 1 calc PR A 1 H21C H 0.1114 0.8569 0.2092 0.176 Uiso 0.60(2) 1 calc PR A 1 C20A C 0.120(3) 0.851(3) 0.2319(15) 0.117(9) Uiso 0.40(2) 1 d PDU A 2 H20D H 0.0722 0.8383 0.2151 0.175 Uiso 0.40(2) 1 calc PR A 2 H20E H 0.1627 0.8601 0.2101 0.175 Uiso 0.40(2) 1 calc PR A 2 H20F H 0.1140 0.9100 0.2503 0.175 Uiso 0.40(2) 1 calc PR A 2 C21A C 0.2009(19) 0.772(3) 0.2964(12) 0.102(9) Uani 0.40(2) 1 d PDU A 2 H21D H 0.1974 0.7148 0.3164 0.153 Uiso 0.40(2) 1 calc PR A 2 H21E H 0.1964 0.8304 0.3149 0.153 Uiso 0.40(2) 1 calc PR A 2 H21F H 0.2508 0.7713 0.2805 0.153 Uiso 0.40(2) 1 calc PR A 2 C22 C -0.0886(9) 0.7729(12) 0.0929(6) 0.107(5) Uani 1 1 d DU . . H22 H -0.1027 0.7626 0.0601 0.128 Uiso 0.80(2) 1 calc PR B 1 H22A H -0.1345 0.7764 0.1137 0.128 Uiso 0.20(2) 1 calc PR B 2 C23 C -0.0245(12) 0.8473(13) 0.0926(9) 0.114(6) Uani 0.80(2) 1 d PDU B 1 H23A H 0.0182 0.8243 0.0734 0.171 Uiso 0.80(2) 1 calc PR B 1 H23B H -0.0058 0.8574 0.1240 0.171 Uiso 0.80(2) 1 calc PR B 1 H23C H -0.0443 0.9083 0.0803 0.171 Uiso 0.80(2) 1 calc PR B 1 C24 C -0.1624(11) 0.8027(16) 0.1165(8) 0.117(6) Uani 0.80(2) 1 d PDU B 1 H24A H -0.2017 0.7526 0.1121 0.175 Uiso 0.80(2) 1 calc PR B 1 H24B H -0.1808 0.8638 0.1034 0.175 Uiso 0.80(2) 1 calc PR B 1 H24C H -0.1526 0.8112 0.1493 0.175 Uiso 0.80(2) 1 calc PR B 1 C23A C -0.042(5) 0.852(4) 0.116(3) 0.110(9) Uiso 0.20(2) 1 d PDU B 2 H23D H 0.0130 0.8395 0.1117 0.166 Uiso 0.20(2) 1 calc PR B 2 H23E H -0.0541 0.8523 0.1489 0.166 Uiso 0.20(2) 1 calc PR B 2 H23F H -0.0558 0.9143 0.1027 0.166 Uiso 0.20(2) 1 calc PR B 2 C24A C -0.130(5) 0.802(5) 0.0497(18) 0.107(11) Uani 0.20(2) 1 d PDU B 2 H24D H -0.1794 0.7667 0.0477 0.161 Uiso 0.20(2) 1 calc PR B 2 H24E H -0.0981 0.7856 0.0231 0.161 Uiso 0.20(2) 1 calc PR B 2 H24F H -0.1402 0.8713 0.0501 0.161 Uiso 0.20(2) 1 calc PR B 2 C25 C -0.1276(9) 0.5645(12) 0.1000(5) 0.094(4) Uani 1 1 d DU . . H25 H -0.1778 0.5872 0.1131 0.113 Uiso 0.626(15) 1 calc PR B 1 H25A H -0.1571 0.5884 0.0728 0.113 Uiso 0.374(15) 1 calc PR B 2 C26 C -0.1406(14) 0.538(2) 0.0502(7) 0.106(6) Uani 0.626(15) 1 d PDU B 1 H26A H -0.1559 0.5964 0.0331 0.160 Uiso 0.626(15) 1 calc PR B 1 H26B H -0.1817 0.4899 0.0481 0.160 Uiso 0.626(15) 1 calc PR B 1 H26C H -0.0928 0.5122 0.0372 0.160 Uiso 0.626(15) 1 calc PR B 1 C27 C -0.1039(17) 0.4730(16) 0.1250(9) 0.116(7) Uani 0.626(15) 1 d PDU B 1 H27A H -0.0952 0.4876 0.1574 0.174 Uiso 0.626(15) 1 calc PR B 1 H27B H -0.0561 0.4476 0.1115 0.174 Uiso 0.626(15) 1 calc PR B 1 H27C H -0.1450 0.4246 0.1221 0.174 Uiso 0.626(15) 1 calc PR B 1 C26A C -0.096(2) 0.4658(18) 0.0881(15) 0.107(7) Uani 0.374(15) 1 d PDU B 2 H26D H -0.0578 0.4721 0.0633 0.161 Uiso 0.374(15) 1 calc PR B 2 H26E H -0.1381 0.4237 0.0781 0.161 Uiso 0.374(15) 1 calc PR B 2 H26F H -0.0707 0.4377 0.1151 0.161 Uiso 0.374(15) 1 calc PR B 2 C27A C -0.1844(17) 0.553(3) 0.1390(10) 0.100(8) Uani 0.374(15) 1 d PDU B 2 H27D H -0.2041 0.6166 0.1480 0.150 Uiso 0.374(15) 1 calc PR B 2 H27E H -0.1584 0.5229 0.1652 0.150 Uiso 0.374(15) 1 calc PR B 2 H27F H -0.2275 0.5121 0.1291 0.150 Uiso 0.374(15) 1 calc PR B 2 P3 P 0.6193(2) 0.6587(3) 0.04480(16) 0.0929(12) Uani 1 1 d DU . . F1 F 0.5567(7) 0.5772(9) 0.0420(5) 0.138(4) Uani 0.605(9) 1 d PDU C 1 F2 F 0.6786(7) 0.5846(9) 0.0640(5) 0.156(4) Uani 0.605(9) 1 d PDU C 1 F3 F 0.5952(9) 0.6876(11) 0.0940(3) 0.149(4) Uani 0.605(9) 1 d PDU C 1 F4 F 0.6825(7) 0.7410(9) 0.0446(6) 0.145(4) Uani 0.605(9) 1 d PDU C 1 F5 F 0.5602(7) 0.7344(8) 0.0236(5) 0.129(4) Uani 0.605(9) 1 d PDU C 1 F6 F 0.6431(8) 0.6324(10) -0.0066(3) 0.133(4) Uani 0.605(9) 1 d PDU C 1 F1A F 0.6762(9) 0.6971(15) 0.0077(6) 0.147(5) Uani 0.395(9) 1 d PDU C 2 F2A F 0.5819(10) 0.7619(8) 0.0479(7) 0.135(5) Uani 0.395(9) 1 d PDU C 2 F3A F 0.5574(9) 0.6306(15) 0.0077(6) 0.136(4) Uani 0.395(9) 1 d PDU C 2 F4A F 0.5615(9) 0.6195(15) 0.0828(6) 0.128(5) Uani 0.395(9) 1 d PDU C 2 F5A F 0.6558(11) 0.5547(8) 0.0421(7) 0.141(5) Uani 0.395(9) 1 d PDU C 2 F6A F 0.6795(9) 0.6850(15) 0.0831(6) 0.137(4) Uani 0.395(9) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0437(5) 0.0442(5) 0.0726(7) -0.0040(5) 0.0034(5) -0.0040(4) Pd 0.0456(5) 0.0660(6) 0.0455(5) -0.0022(5) 0.0094(4) -0.0045(4) Cl 0.073(2) 0.154(4) 0.082(3) -0.010(3) 0.032(2) 0.011(2) P1 0.066(2) 0.081(2) 0.0443(18) 0.0015(18) 0.0010(16) -0.0109(19) P2 0.0416(17) 0.069(2) 0.0576(19) -0.0024(17) -0.0015(14) 0.0006(15) O1 0.059(6) 0.138(9) 0.051(5) 0.007(5) -0.005(4) -0.010(5) O2 0.045(5) 0.117(8) 0.055(5) -0.003(5) -0.003(4) -0.004(5) C1 0.055(7) 0.052(7) 0.051(7) 0.003(6) 0.002(6) -0.008(6) C2 0.031(6) 0.061(7) 0.042(6) -0.004(5) 0.004(5) 0.005(5) C3 0.043(6) 0.055(7) 0.043(6) -0.007(5) 0.010(5) -0.002(5) C4 0.061(8) 0.078(9) 0.039(6) -0.012(6) -0.001(6) -0.021(7) C5 0.051(7) 0.065(8) 0.085(9) -0.027(7) 0.008(7) 0.003(6) C6 0.061(5) 0.064(5) 0.104(6) 0.008(5) 0.016(5) 0.001(4) C7 0.061(5) 0.064(5) 0.104(6) 0.008(5) 0.016(5) 0.001(4) C8 0.061(5) 0.064(5) 0.104(6) 0.008(5) 0.016(5) 0.001(4) C9 0.050(7) 0.038(6) 0.076(8) -0.009(6) 0.011(6) -0.007(5) C10 0.051(7) 0.039(6) 0.051(7) -0.006(5) 0.007(5) -0.006(5) C11 0.088(9) 0.031(5) 0.186(15) 0.012(8) 0.034(8) 0.004(5) C12 0.072(10) 0.044(8) 0.20(2) -0.008(10) 0.050(12) -0.021(7) C13 0.141(14) 0.085(8) 0.142(14) -0.030(9) -0.037(11) -0.031(11) C14 0.141(14) 0.085(8) 0.142(14) -0.030(9) -0.037(11) -0.031(11) C15 0.088(9) 0.031(5) 0.186(15) 0.012(8) 0.034(8) 0.004(5) C16 0.089(9) 0.123(10) 0.069(8) 0.018(8) -0.012(6) -0.008(9) C17 0.098(14) 0.157(18) 0.065(14) 0.035(13) -0.015(11) -0.003(13) C18 0.106(17) 0.111(13) 0.104(13) 0.018(11) -0.015(14) -0.004(13) C17A 0.103(18) 0.118(13) 0.098(14) 0.016(11) -0.012(14) -0.006(15) C18A 0.107(17) 0.137(18) 0.077(16) 0.024(14) 0.005(11) -0.019(16) C19 0.117(10) 0.105(9) 0.090(9) -0.007(7) -0.016(7) -0.017(9) C20 0.140(18) 0.119(17) 0.103(15) -0.008(13) -0.001(11) 0.001(15) C21 0.125(15) 0.107(13) 0.120(12) -0.001(10) -0.008(11) -0.039(12) C21A 0.111(18) 0.096(18) 0.098(18) -0.028(16) -0.016(12) -0.035(17) C22 0.107(9) 0.085(9) 0.129(10) 0.029(8) -0.016(8) 0.016(7) C23 0.120(11) 0.089(11) 0.134(13) 0.031(11) 0.003(11) 0.008(8) C24 0.095(10) 0.106(13) 0.149(16) 0.003(12) -0.027(10) 0.015(10) C24A 0.10(2) 0.09(2) 0.13(2) 0.02(2) -0.026(17) 0.01(2) C25 0.072(8) 0.117(10) 0.092(9) -0.033(8) -0.005(7) -0.017(8) C26 0.089(13) 0.131(15) 0.099(11) -0.041(11) -0.020(11) -0.035(12) C27 0.114(14) 0.115(13) 0.119(14) -0.025(11) -0.026(13) -0.027(12) C26A 0.095(13) 0.115(13) 0.111(15) -0.034(13) -0.007(13) -0.015(11) C27A 0.061(16) 0.14(2) 0.102(17) -0.033(15) -0.005(11) -0.035(14) P3 0.065(2) 0.100(3) 0.114(3) -0.011(3) 0.008(2) 0.0035(19) F1 0.102(7) 0.149(8) 0.163(10) 0.007(8) -0.003(7) -0.040(6) F2 0.117(7) 0.144(8) 0.208(9) -0.007(8) -0.046(8) 0.030(6) F3 0.155(9) 0.183(10) 0.109(5) -0.017(6) -0.001(6) 0.019(7) F4 0.125(7) 0.146(8) 0.163(10) -0.023(8) -0.024(7) -0.045(6) F5 0.118(7) 0.137(8) 0.132(8) -0.013(7) -0.020(7) 0.033(6) F6 0.112(9) 0.149(10) 0.136(5) -0.046(6) 0.029(6) -0.016(7) F1A 0.125(9) 0.159(11) 0.156(9) -0.016(9) 0.052(7) -0.022(8) F2A 0.138(10) 0.118(6) 0.150(11) -0.016(7) 0.011(8) 0.030(7) F3A 0.111(8) 0.161(10) 0.138(8) -0.021(8) -0.024(6) -0.003(8) F4A 0.104(9) 0.149(10) 0.132(8) -0.012(9) 0.018(7) -0.035(8) F5A 0.141(11) 0.119(7) 0.164(13) -0.022(7) -0.012(9) 0.034(7) F6A 0.102(8) 0.151(10) 0.158(8) -0.016(8) -0.026(6) -0.024(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C7 2.132(13) . ? Ru C12 2.133(13) . ? Ru C15 2.140(13) . ? Ru C14 2.143(17) . ? Ru C8 2.161(13) . ? Ru C5 2.175(12) . ? Ru C11 2.175(15) . ? Ru C13 2.188(17) . ? Ru C6 2.213(14) . ? Ru C9 2.250(11) . ? Ru C10 2.294(10) . ? Pd C2 1.950(9) . ? Pd P1 2.272(4) . ? Pd P2 2.284(3) . ? Pd Cl 2.367(3) . ? P1 O1 1.647(9) . ? P1 C16 1.812(15) . ? P1 C19 1.824(16) . ? P2 O2 1.654(8) . ? P2 C22 1.800(15) . ? P2 C25 1.816(15) . ? O1 C1 1.411(13) . ? O2 C3 1.346(12) . ? C1 C2 1.339(14) . ? C1 C9 1.424(15) . ? C2 C3 1.487(14) . ? C3 C4 1.321(14) . ? C4 C10 1.450(15) . ? C5 C6 1.381(17) . ? C5 C10 1.438(15) . ? C6 C7 1.335(19) . ? C7 C8 1.360(17) . ? C8 C9 1.413(16) . ? C9 C10 1.410(15) . ? C11 C15 1.39(2) . ? C11 C12 1.40(2) . ? C12 C13 1.44(3) . ? C13 C14 1.41(3) . ? C14 C15 1.37(2) . ? C16 C18A 1.514(16) . ? C16 C17A 1.516(16) . ? C16 C17 1.519(15) . ? C16 C18 1.520(16) . ? C19 C20 1.439(16) . ? C19 C21A 1.446(16) . ? C19 C21 1.450(16) . ? C19 C20A 1.451(16) . ? C22 C24A 1.476(17) . ? C22 C24 1.477(16) . ? C22 C23A 1.481(17) . ? C22 C23 1.482(16) . ? C25 C27A 1.482(16) . ? C25 C26A 1.482(16) . ? C25 C26 1.483(15) . ? C25 C27 1.488(16) . ? P3 F3 1.517(7) . ? P3 F2 1.524(7) . ? P3 F1A 1.527(7) . ? P3 F1 1.534(7) . ? P3 F2A 1.538(7) . ? P3 F6A 1.538(7) . ? P3 F3A 1.541(7) . ? P3 F5A 1.543(7) . ? P3 F4 1.546(7) . ? P3 F4A 1.556(7) . ? P3 F5 1.556(7) . ? P3 F6 1.566(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ru C12 122.3(6) . . ? C7 Ru C15 158.9(7) . . ? C12 Ru C15 62.8(6) . . ? C7 Ru C14 123.3(7) . . ? C12 Ru C14 63.3(8) . . ? C15 Ru C14 37.4(6) . . ? C7 Ru C8 36.9(4) . . ? C12 Ru C8 149.6(7) . . ? C15 Ru C8 127.5(6) . . ? C14 Ru C8 106.4(7) . . ? C7 Ru C5 64.6(5) . . ? C12 Ru C5 116.4(6) . . ? C15 Ru C5 134.2(6) . . ? C14 Ru C5 171.5(7) . . ? C8 Ru C5 78.1(5) . . ? C7 Ru C11 157.8(6) . . ? C12 Ru C11 38.0(6) . . ? C15 Ru C11 37.7(6) . . ? C14 Ru C11 63.4(8) . . ? C8 Ru C11 164.9(6) . . ? C5 Ru C11 110.7(6) . . ? C7 Ru C13 106.6(7) . . ? C12 Ru C13 38.8(7) . . ? C15 Ru C13 63.5(7) . . ? C14 Ru C13 37.9(7) . . ? C8 Ru C13 115.0(7) . . ? C5 Ru C13 146.9(7) . . ? C11 Ru C13 64.6(7) . . ? C7 Ru C6 35.7(5) . . ? C12 Ru C6 108.2(5) . . ? C15 Ru C6 165.1(7) . . ? C14 Ru C6 151.7(7) . . ? C8 Ru C6 66.5(5) . . ? C5 Ru C6 36.7(4) . . ? C11 Ru C6 128.0(6) . . ? C13 Ru C6 117.9(7) . . ? C7 Ru C9 66.0(4) . . ? C12 Ru C9 171.6(5) . . ? C15 Ru C9 109.4(5) . . ? C14 Ru C9 113.0(7) . . ? C8 Ru C9 37.3(4) . . ? C5 Ru C9 66.0(4) . . ? C11 Ru C9 133.8(5) . . ? C13 Ru C9 142.5(7) . . ? C6 Ru C9 78.7(4) . . ? C7 Ru C10 77.3(5) . . ? C12 Ru C10 141.5(7) . . ? C15 Ru C10 111.8(5) . . ? C14 Ru C10 137.3(7) . . ? C8 Ru C10 66.3(5) . . ? C5 Ru C10 37.4(4) . . ? C11 Ru C10 112.8(5) . . ? C13 Ru C10 175.0(7) . . ? C6 Ru C10 67.0(4) . . ? C9 Ru C10 36.1(4) . . ? C2 Pd P1 80.0(3) . . ? C2 Pd P2 81.2(3) . . ? P1 Pd P2 160.92(12) . . ? C2 Pd Cl 177.4(3) . . ? P1 Pd Cl 98.36(14) . . ? P2 Pd Cl 100.55(13) . . ? O1 P1 C16 101.0(6) . . ? O1 P1 C19 102.3(7) . . ? C16 P1 C19 109.4(7) . . ? O1 P1 Pd 103.8(3) . . ? C16 P1 Pd 121.3(5) . . ? C19 P1 Pd 115.6(5) . . ? O2 P2 C22 100.6(6) . . ? O2 P2 C25 103.3(6) . . ? C22 P2 C25 107.2(7) . . ? O2 P2 Pd 103.9(3) . . ? C22 P2 Pd 117.8(6) . . ? C25 P2 Pd 120.9(5) . . ? C1 O1 P1 114.3(7) . . ? C3 O2 P2 117.3(7) . . ? C2 C1 O1 117.5(10) . . ? C2 C1 C9 126.7(11) . . ? O1 C1 C9 115.8(10) . . ? C1 C2 C3 114.5(9) . . ? C1 C2 Pd 124.3(8) . . ? C3 C2 Pd 121.2(7) . . ? C4 C3 O2 120.3(10) . . ? C4 C3 C2 123.5(10) . . ? O2 C3 C2 116.2(9) . . ? C3 C4 C10 118.5(10) . . ? C6 C5 C10 124.0(13) . . ? C6 C5 Ru 73.2(8) . . ? C10 C5 Ru 75.8(6) . . ? C7 C6 C5 115.7(13) . . ? C7 C6 Ru 68.8(8) . . ? C5 C6 Ru 70.1(7) . . ? C6 C7 C8 125.7(14) . . ? C6 C7 Ru 75.5(9) . . ? C8 C7 Ru 72.7(8) . . ? C7 C8 C9 119.0(14) . . ? C7 C8 Ru 70.4(8) . . ? C9 C8 Ru 74.8(7) . . ? C10 C9 C8 119.5(11) . . ? C10 C9 C1 115.2(10) . . ? C8 C9 C1 125.2(12) . . ? C10 C9 Ru 73.6(6) . . ? C8 C9 Ru 67.9(7) . . ? C1 C9 Ru 128.3(8) . . ? C9 C10 C5 115.7(10) . . ? C9 C10 C4 121.4(10) . . ? C5 C10 C4 122.8(10) . . ? C9 C10 Ru 70.3(6) . . ? C5 C10 Ru 66.8(6) . . ? C4 C10 Ru 130.6(8) . . ? C15 C11 C12 105.5(18) . . ? C15 C11 Ru 69.8(9) . . ? C12 C11 Ru 69.3(9) . . ? C11 C12 C13 110.4(17) . . ? C11 C12 Ru 72.6(8) . . ? C13 C12 Ru 72.7(10) . . ? C14 C13 C12 104.1(19) . . ? C14 C13 Ru 69.3(11) . . ? C12 C13 Ru 68.5(9) . . ? C15 C14 C13 110(2) . . ? C15 C14 Ru 71.2(9) . . ? C13 C14 Ru 72.8(11) . . ? C14 C15 C11 110.1(18) . . ? C14 C15 Ru 71.4(9) . . ? C11 C15 Ru 72.5(8) . . ? C18A C16 C17A 111.2(18) . . ? C18A C16 C17 112(2) . . ? C17A C16 C17 91(2) . . ? C18A C16 C18 92(2) . . ? C17 C16 C18 110.5(17) . . ? C18A C16 P1 111.0(16) . . ? C17A C16 P1 111(2) . . ? C17 C16 P1 119.8(14) . . ? C18 C16 P1 108.3(17) . . ? C20 C19 C21A 88(2) . . ? C20 C19 C21 123(2) . . ? C21A C19 C21 107(2) . . ? C20 C19 C20A 99(3) . . ? C21A C19 C20A 122(2) . . ? C20 C19 P1 110.1(16) . . ? C21A C19 P1 118.1(18) . . ? C21 C19 P1 110.0(15) . . ? C20A C19 P1 113(2) . . ? C24A C22 C24 85(4) . . ? C24A C22 C23A 116(2) . . ? C24 C22 C23A 93(4) . . ? C24A C22 C23 100(3) . . ? C24 C22 C23 115.9(17) . . ? C24A C22 P2 132(3) . . ? C24 C22 P2 112.3(13) . . ? C23A C22 P2 108(3) . . ? C23 C22 P2 110.7(12) . . ? C27A C25 C26A 108.3(18) . . ? C27A C25 C26 127(2) . . ? C26A C25 C26 67.6(18) . . ? C27A C25 C27 74.1(19) . . ? C26 C25 C27 107.6(16) . . ? C27A C25 P2 111.4(16) . . ? C26A C25 P2 114.2(19) . . ? C26 C25 P2 118.2(13) . . ? C27 C25 P2 106.1(13) . . ? F3 P3 F2 90.7(5) . . ? F3 P3 F1A 136.7(8) . . ? F2 P3 F1A 93.4(10) . . ? F3 P3 F1 92.8(5) . . ? F2 P3 F1 90.0(5) . . ? F1A P3 F1 130.2(7) . . ? F3 P3 F2A 66.5(8) . . ? F2 P3 F2A 148.3(7) . . ? F1A P3 F2A 89.5(5) . . ? F1 P3 F2A 111.9(8) . . ? F3 P3 F6A 57.2(7) . . ? F2 P3 F6A 57.2(7) . . ? F1A P3 F6A 89.8(5) . . ? F1 P3 F6A 131.5(7) . . ? F2A P3 F6A 91.2(6) . . ? F3 P3 F3A 121.4(7) . . ? F2 P3 F3A 122.3(7) . . ? F1A P3 F3A 92.0(6) . . ? F1 P3 F3A 46.7(7) . . ? F2A P3 F3A 89.1(5) . . ? F6A P3 F3A 178.2(5) . . ? F3 P3 F5A 112.9(8) . . ? F1A P3 F5A 91.3(5) . . ? F1 P3 F5A 67.4(8) . . ? F2A P3 F5A 179.2(6) . . ? F6A P3 F5A 88.9(5) . . ? F3A P3 F5A 90.7(5) . . ? F3 P3 F4 90.2(5) . . ? F2 P3 F4 91.2(5) . . ? F1 P3 F4 176.8(5) . . ? F2A P3 F4 68.2(9) . . ? F6A P3 F4 51.4(7) . . ? F3A P3 F4 130.3(7) . . ? F5A P3 F4 112.5(9) . . ? F2 P3 F4A 86.4(10) . . ? F1A P3 F4A 179.8(6) . . ? F2A P3 F4A 90.7(5) . . ? F6A P3 F4A 90.0(5) . . ? F3A P3 F4A 88.2(5) . . ? F5A P3 F4A 88.5(5) . . ? F4 P3 F4A 133.2(7) . . ? F3 P3 F5 91.1(5) . . ? F2 P3 F5 178.0(5) . . ? F1A P3 F5 84.8(9) . . ? F1 P3 F5 90.6(5) . . ? F6A P3 F5 123.5(7) . . ? F3A P3 F5 57.1(7) . . ? F5A P3 F5 147.3(7) . . ? F4 P3 F5 88.2(5) . . ? F4A P3 F5 95.4(9) . . ? F3 P3 F6 178.1(5) . . ? F2 P3 F6 91.0(5) . . ? F1 P3 F6 87.9(5) . . ? F2A P3 F6 111.6(8) . . ? F6A P3 F6 123.4(7) . . ? F3A P3 F6 58.1(7) . . ? F5A P3 F6 69.0(8) . . ? F4 P3 F6 89.0(5) . . ? F4A P3 F6 137.7(8) . . ? F5 P3 F6 87.1(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.316 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.140 #============================================================================== data_compound-4c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl O2 P2 Pt Ru, F6 P' _chemical_formula_sum 'C54 H76 Cl2 F12 O4 P6 Pt2 Ru2' _chemical_formula_weight 1866.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.832(1) _cell_length_b 13.431(1) _cell_length_c 28.285(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.051(1) _cell_angle_gamma 90.00 _cell_volume 6394.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7421 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 5.137 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4583 _exptl_absorpt_correction_T_max 0.8209 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36805 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12947 _reflns_number_gt 11853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Crystal were found to be twinned ; twin fraction 0.58/0.42 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+36.1436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12947 _refine_ls_number_parameters 756 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.518280(19) 0.15236(2) 0.185719(16) 0.02657(9) Uani 1 1 d . . . Ru1 Ru 0.83206(4) 0.20576(5) 0.09078(3) 0.02395(16) Uani 1 1 d . . . Cl1 Cl 0.41695(16) 0.1681(2) 0.24366(11) 0.0452(7) Uani 1 1 d . . . P1 P 0.44673(14) 0.17193(19) 0.11830(10) 0.0277(6) Uani 1 1 d . . . P2 P 0.62232(15) 0.1401(2) 0.23626(10) 0.0279(6) Uani 1 1 d . . . O1 O 0.5120(4) 0.1609(5) 0.0759(2) 0.0369(16) Uani 1 1 d . . . O2 O 0.6968(4) 0.1093(5) 0.2011(2) 0.0307(16) Uani 1 1 d . . . C1 C 0.6047(6) 0.1328(7) 0.1394(4) 0.026(2) Uani 1 1 d . . . C2 C 0.5894(5) 0.1409(6) 0.0897(4) 0.027(2) Uani 1 1 d . . . C3 C 0.6461(5) 0.1295(7) 0.0558(3) 0.026(2) Uani 1 1 d . . . H3 H 0.6336 0.1373 0.0233 0.032 Uiso 1 1 calc R . . C4 C 0.7242(5) 0.1056(7) 0.0706(4) 0.026(2) Uani 1 1 d . . . C5 C 0.7435(5) 0.0957(6) 0.1211(3) 0.0201(18) Uani 1 1 d . . . C6 C 0.6813(5) 0.1125(7) 0.1536(3) 0.023(2) Uani 1 1 d . . . C7 C 0.7886(5) 0.0960(7) 0.0380(4) 0.029(2) Uani 1 1 d . . . H7 H 0.7792 0.1082 0.0054 0.035 Uiso 1 1 calc R . . C8 C 0.8661(6) 0.0687(8) 0.0529(4) 0.034(2) Uani 1 1 d . . . H8 H 0.9071 0.0595 0.0303 0.040 Uiso 1 1 calc R . . C9 C 0.8818(6) 0.0553(6) 0.1007(4) 0.034(2) Uani 1 1 d . . . H9 H 0.9331 0.0339 0.1105 0.041 Uiso 1 1 calc R . . C10 C 0.8226(5) 0.0733(6) 0.1352(4) 0.024(2) Uani 1 1 d . . . H10 H 0.8357 0.0704 0.1679 0.029 Uiso 1 1 calc R . . C11 C 0.4079(6) 0.2966(7) 0.1093(4) 0.037(3) Uani 1 1 d . . . H11 H 0.3661 0.3077 0.1339 0.044 Uiso 1 1 calc R . . C12 C 0.4744(7) 0.3734(6) 0.1185(4) 0.045(3) Uani 1 1 d . . . H12A H 0.5192 0.3600 0.0974 0.067 Uiso 1 1 calc R . . H12B H 0.4921 0.3682 0.1514 0.067 Uiso 1 1 calc R . . H12C H 0.4540 0.4406 0.1126 0.067 Uiso 1 1 calc R . . C13 C 0.3710(8) 0.3160(9) 0.0630(5) 0.064(4) Uani 1 1 d . . . H13A H 0.3604 0.3874 0.0598 0.096 Uiso 1 1 calc R . . H13B H 0.3210 0.2789 0.0607 0.096 Uiso 1 1 calc R . . H13C H 0.4070 0.2944 0.0378 0.096 Uiso 1 1 calc R . . C14 C 0.3720(5) 0.0810(7) 0.1001(4) 0.031(2) Uani 1 1 d . . . H14 H 0.3478 0.1032 0.0696 0.037 Uiso 1 1 calc R . . C15 C 0.4115(8) -0.0193(8) 0.0927(6) 0.062(4) Uani 1 1 d . . . H15A H 0.4556 -0.0267 0.1151 0.093 Uiso 1 1 calc R . . H15B H 0.4318 -0.0234 0.0603 0.093 Uiso 1 1 calc R . . H15C H 0.3726 -0.0724 0.0980 0.093 Uiso 1 1 calc R . . C16 C 0.3069(6) 0.0761(9) 0.1378(5) 0.054(3) Uani 1 1 d . . . H16A H 0.2699 0.0221 0.1302 0.082 Uiso 1 1 calc R . . H16B H 0.2781 0.1395 0.1385 0.082 Uiso 1 1 calc R . . H16C H 0.3311 0.0637 0.1688 0.082 Uiso 1 1 calc R . . C17 C 0.6583(7) 0.2540(8) 0.2639(4) 0.042(3) Uani 1 1 d . . . H17 H 0.7111 0.2393 0.2786 0.050 Uiso 1 1 calc R . . C18 C 0.6709(8) 0.3315(8) 0.2255(5) 0.064(4) Uani 1 1 d . . . H18A H 0.6194 0.3522 0.2128 0.096 Uiso 1 1 calc R . . H18B H 0.7033 0.3029 0.2001 0.096 Uiso 1 1 calc R . . H18C H 0.6983 0.3894 0.2389 0.096 Uiso 1 1 calc R . . C19 C 0.6025(8) 0.2866(9) 0.3027(5) 0.063(4) Uani 1 1 d . . . H19A H 0.6268 0.3413 0.3206 0.094 Uiso 1 1 calc R . . H19B H 0.5923 0.2305 0.3240 0.094 Uiso 1 1 calc R . . H19C H 0.5524 0.3092 0.2888 0.094 Uiso 1 1 calc R . . C20 C 0.6215(6) 0.0431(8) 0.2808(4) 0.034(2) Uani 1 1 d . . . H20 H 0.5767 0.0582 0.3029 0.041 Uiso 1 1 calc R . . C21 C 0.6031(8) -0.0568(9) 0.2576(5) 0.055(3) Uani 1 1 d . . . H21A H 0.6424 -0.0703 0.2329 0.082 Uiso 1 1 calc R . . H21B H 0.5499 -0.0546 0.2436 0.082 Uiso 1 1 calc R . . H21C H 0.6052 -0.1096 0.2815 0.082 Uiso 1 1 calc R . . C22 C 0.6975(6) 0.0388(8) 0.3106(4) 0.049(3) Uani 1 1 d . . . H22A H 0.6945 -0.0175 0.3326 0.074 Uiso 1 1 calc R . . H22B H 0.7032 0.1009 0.3285 0.074 Uiso 1 1 calc R . . H22C H 0.7435 0.0303 0.2898 0.074 Uiso 1 1 calc R . . C23 C 0.8664(7) 0.3236(7) 0.1378(5) 0.047(3) Uani 1 1 d . . . H23 H 0.8700 0.3130 0.1709 0.057 Uiso 1 1 calc R . . C24 C 0.7988(7) 0.3555(6) 0.1139(4) 0.046(3) Uani 1 1 d . . . H24 H 0.7495 0.3731 0.1280 0.055 Uiso 1 1 calc R . . C25 C 0.8167(6) 0.3570(6) 0.0641(4) 0.039(3) Uani 1 1 d . . . H25 H 0.7815 0.3737 0.0390 0.046 Uiso 1 1 calc R . . C26 C 0.8983(6) 0.3281(7) 0.0599(4) 0.036(2) Uani 1 1 d . . . H26 H 0.9274 0.3225 0.0312 0.043 Uiso 1 1 calc R . . C27 C 0.9282(7) 0.3094(7) 0.1058(4) 0.040(3) Uani 1 1 d . . . H27 H 0.9810 0.2905 0.1134 0.048 Uiso 1 1 calc R . . Pt2 Pt 0.002439(18) 0.16471(2) 0.317326(13) 0.02218(8) Uani 1 1 d . . . Ru2 Ru 0.32462(4) 0.21227(5) 0.40594(3) 0.02447(16) Uani 1 1 d . . . Cl2 Cl -0.10745(14) 0.1847(2) 0.26560(10) 0.0342(6) Uani 1 1 d . . . P3 P 0.10094(15) 0.16662(18) 0.26302(9) 0.0237(5) Uani 1 1 d . . . P4 P -0.06266(14) 0.15703(17) 0.38738(9) 0.0234(5) Uani 1 1 d . . . O3 O 0.1841(4) 0.1468(5) 0.2942(2) 0.0295(15) Uani 1 1 d . . . O4 O 0.0084(4) 0.1331(5) 0.4270(2) 0.0293(14) Uani 1 1 d . . . C28 C 0.0942(6) 0.1412(7) 0.3595(3) 0.024(2) Uani 1 1 d . . . C29 C 0.1685(5) 0.1339(7) 0.3422(3) 0.0226(19) Uani 1 1 d . . . C30 C 0.2367(5) 0.1083(6) 0.3703(3) 0.0210(18) Uani 1 1 d . . . C31 C 0.2245(5) 0.1002(6) 0.4204(4) 0.025(2) Uani 1 1 d . . . C32 C 0.1457(5) 0.1112(6) 0.4399(3) 0.024(2) Uani 1 1 d . . . H32 H 0.1367 0.1067 0.4730 0.029 Uiso 1 1 calc R . . C33 C 0.0851(5) 0.1279(6) 0.4096(3) 0.0204(18) Uani 1 1 d . . . C34 C 0.3151(5) 0.0972(7) 0.3521(4) 0.033(2) Uani 1 1 d . . . H34 H 0.3244 0.1066 0.3193 0.040 Uiso 1 1 calc R . . C35 C 0.3780(6) 0.0729(7) 0.3816(4) 0.028(2) Uani 1 1 d . . . H35 H 0.4291 0.0613 0.3686 0.034 Uiso 1 1 calc R . . C36 C 0.3663(6) 0.0654(7) 0.4310(4) 0.033(2) Uani 1 1 d . . . H36 H 0.4095 0.0481 0.4510 0.039 Uiso 1 1 calc R . . C37 C 0.2914(6) 0.0832(6) 0.4503(3) 0.026(2) Uani 1 1 d . . . H37 H 0.2849 0.0840 0.4837 0.031 Uiso 1 1 calc R . . C38 C 0.1224(6) 0.2843(6) 0.2335(4) 0.029(2) Uani 1 1 d . . . H38 H 0.0769 0.2998 0.2120 0.034 Uiso 1 1 calc R . . C39 C 0.1273(7) 0.3683(7) 0.2714(4) 0.048(3) Uani 1 1 d . . . H39A H 0.1759 0.3600 0.2902 0.072 Uiso 1 1 calc R . . H39B H 0.0809 0.3644 0.2922 0.072 Uiso 1 1 calc R . . H39C H 0.1282 0.4333 0.2557 0.072 Uiso 1 1 calc R . . C40 C 0.1989(6) 0.2803(8) 0.2032(4) 0.049(3) Uani 1 1 d . . . H40A H 0.2133 0.3478 0.1932 0.074 Uiso 1 1 calc R . . H40B H 0.1895 0.2388 0.1752 0.074 Uiso 1 1 calc R . . H40C H 0.2423 0.2518 0.2219 0.074 Uiso 1 1 calc R . . C41 C 0.1089(6) 0.0677(7) 0.2196(4) 0.032(2) Uani 1 1 d . . . H41 H 0.1610 0.0734 0.2027 0.039 Uiso 1 1 calc R . . C42 C 0.0410(7) 0.0776(8) 0.1837(4) 0.053(3) Uani 1 1 d . . . H42A H 0.0246 0.0113 0.1731 0.080 Uiso 1 1 calc R . . H42B H 0.0591 0.1166 0.1565 0.080 Uiso 1 1 calc R . . H42C H -0.0041 0.1113 0.1987 0.080 Uiso 1 1 calc R . . C43 C 0.1048(7) -0.0337(7) 0.2454(4) 0.045(3) Uani 1 1 d . . . H43A H 0.0511 -0.0437 0.2579 0.068 Uiso 1 1 calc R . . H43B H 0.1431 -0.0343 0.2715 0.068 Uiso 1 1 calc R . . H43C H 0.1175 -0.0873 0.2231 0.068 Uiso 1 1 calc R . . C44 C -0.1083(6) 0.2698(7) 0.4108(4) 0.036(2) Uani 1 1 d . . . H44 H -0.1272 0.2553 0.4436 0.044 Uiso 1 1 calc R . . C45 C -0.0453(9) 0.3497(8) 0.4138(5) 0.061(4) Uani 1 1 d . . . H45A H -0.0210 0.3590 0.3827 0.092 Uiso 1 1 calc R . . H45B H -0.0044 0.3296 0.4366 0.092 Uiso 1 1 calc R . . H45C H -0.0696 0.4123 0.4242 0.092 Uiso 1 1 calc R . . C46 C -0.1783(6) 0.3011(8) 0.3819(5) 0.052(3) Uani 1 1 d . . . H46A H -0.1974 0.3660 0.3930 0.078 Uiso 1 1 calc R . . H46B H -0.2207 0.2517 0.3850 0.078 Uiso 1 1 calc R . . H46C H -0.1626 0.3063 0.3486 0.078 Uiso 1 1 calc R . . C47 C -0.1294(6) 0.0530(8) 0.3966(4) 0.036(2) Uani 1 1 d . . . H47 H -0.1799 0.0686 0.3795 0.044 Uiso 1 1 calc R . . C48 C -0.1510(7) 0.0356(10) 0.4481(5) 0.063(4) Uani 1 1 d . . . H48A H -0.1740 -0.0310 0.4517 0.094 Uiso 1 1 calc R . . H48B H -0.1898 0.0857 0.4582 0.094 Uiso 1 1 calc R . . H48C H -0.1031 0.0410 0.4677 0.094 Uiso 1 1 calc R . . C49 C -0.0950(8) -0.0395(8) 0.3741(6) 0.067(4) Uani 1 1 d . . . H49A H -0.0696 -0.0218 0.3440 0.100 Uiso 1 1 calc R . . H49B H -0.1376 -0.0877 0.3682 0.100 Uiso 1 1 calc R . . H49C H -0.0554 -0.0690 0.3953 0.100 Uiso 1 1 calc R . . C50 C 0.3226(7) 0.3453(7) 0.4499(5) 0.045(3) Uani 1 1 d . . . H50 H 0.3030 0.3473 0.4813 0.054 Uiso 1 1 calc R . . C51 C 0.2786(7) 0.3626(7) 0.4101(6) 0.055(4) Uani 1 1 d . . . H51 H 0.2233 0.3766 0.4093 0.065 Uiso 1 1 calc R . . C52 C 0.3290(10) 0.3561(8) 0.3708(5) 0.059(4) Uani 1 1 d . . . H52 H 0.3142 0.3670 0.3388 0.071 Uiso 1 1 calc R . . C53 C 0.4046(8) 0.3309(8) 0.3869(6) 0.066(5) Uani 1 1 d . . . H53 H 0.4504 0.3200 0.3681 0.080 Uiso 1 1 calc R . . C54 C 0.3999(7) 0.3246(8) 0.4373(5) 0.046(3) Uani 1 1 d . . . H54 H 0.4422 0.3090 0.4582 0.055 Uiso 1 1 calc R . . P5 P 0.12383(15) 0.1685(2) 0.03818(11) 0.0332(6) Uani 1 1 d . . . F1 F 0.1246(7) 0.1908(8) 0.0926(3) 0.102(3) Uani 1 1 d . . . F2 F 0.0531(5) 0.0937(6) 0.0432(4) 0.092(3) Uani 1 1 d . . . F3 F 0.1848(4) 0.0788(6) 0.0447(3) 0.066(2) Uani 1 1 d . . . F4 F 0.1941(4) 0.2450(6) 0.0311(3) 0.077(2) Uani 1 1 d . . . F5 F 0.0629(4) 0.2569(5) 0.0298(3) 0.066(2) Uani 1 1 d . . . F6 F 0.1274(5) 0.1492(5) -0.0165(3) 0.063(2) Uani 1 1 d . . . P6 P 0.38640(17) 0.6516(2) 0.04571(12) 0.0399(7) Uani 1 1 d . . . F7 F 0.4362(8) 0.6624(13) 0.0903(4) 0.176(7) Uani 1 1 d . . . F8 F 0.4431(6) 0.5609(9) 0.0359(6) 0.142(5) Uani 1 1 d . . . F9 F 0.4448(6) 0.7188(9) 0.0183(4) 0.129(5) Uani 1 1 d . . . F10 F 0.3280(9) 0.7375(8) 0.0484(6) 0.185(7) Uani 1 1 d . . . F11 F 0.3277(6) 0.5877(11) 0.0765(5) 0.170(7) Uani 1 1 d . . . F12 F 0.3423(7) 0.6274(10) 0.0008(5) 0.149(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02288(16) 0.02982(17) 0.0270(2) 0.00261(16) 0.00435(17) 0.00075(13) Ru1 0.0225(4) 0.0196(3) 0.0298(4) -0.0014(3) 0.0028(3) -0.0006(3) Cl1 0.0349(14) 0.0607(18) 0.0399(17) 0.0042(13) 0.0174(12) 0.0043(12) P1 0.0216(12) 0.0273(12) 0.0343(15) 0.0035(11) -0.0017(10) 0.0005(9) P2 0.0249(13) 0.0347(14) 0.0242(14) 0.0002(11) -0.0003(10) 0.0004(10) O1 0.018(3) 0.057(4) 0.036(4) 0.012(3) 0.002(3) 0.010(3) O2 0.027(4) 0.046(4) 0.019(4) 0.003(3) 0.001(3) -0.004(3) C1 0.024(5) 0.028(5) 0.024(6) 0.004(4) 0.011(4) 0.005(4) C2 0.027(5) 0.020(4) 0.034(6) 0.005(4) 0.000(4) 0.001(4) C3 0.026(5) 0.036(5) 0.017(5) 0.003(4) -0.001(4) -0.004(4) C4 0.024(5) 0.024(5) 0.030(6) -0.003(4) 0.008(4) -0.004(4) C5 0.020(4) 0.023(4) 0.018(5) -0.004(4) 0.002(3) 0.001(3) C6 0.023(5) 0.025(4) 0.021(5) -0.003(4) -0.004(4) 0.003(4) C7 0.021(5) 0.034(5) 0.032(6) -0.005(4) 0.001(4) 0.001(4) C8 0.038(6) 0.035(5) 0.027(6) -0.007(4) 0.009(4) -0.007(4) C9 0.039(6) 0.013(4) 0.050(7) -0.001(4) 0.004(5) -0.003(4) C10 0.030(5) 0.009(4) 0.034(6) 0.001(4) 0.000(4) 0.000(3) C11 0.030(5) 0.025(5) 0.055(7) 0.016(5) -0.012(5) 0.003(4) C12 0.051(7) 0.015(4) 0.068(8) 0.013(5) -0.008(6) -0.005(4) C13 0.068(9) 0.045(7) 0.078(11) 0.008(7) -0.034(8) 0.009(6) C14 0.032(5) 0.025(5) 0.036(6) -0.004(4) -0.001(4) 0.002(4) C15 0.069(8) 0.035(6) 0.082(11) -0.017(7) 0.028(8) -0.011(6) C16 0.030(6) 0.054(7) 0.079(10) -0.018(7) 0.014(6) -0.018(5) C17 0.050(7) 0.037(6) 0.038(7) -0.008(5) 0.004(5) -0.005(5) C18 0.081(9) 0.029(6) 0.081(11) 0.003(6) -0.003(8) -0.030(6) C19 0.079(9) 0.050(7) 0.060(10) -0.018(7) 0.018(7) 0.004(6) C20 0.030(5) 0.040(6) 0.033(6) 0.004(5) 0.000(4) 0.000(4) C21 0.077(9) 0.041(7) 0.045(8) 0.013(6) -0.016(6) -0.006(6) C22 0.042(6) 0.050(6) 0.055(8) 0.018(6) -0.010(6) -0.001(5) C23 0.064(8) 0.022(5) 0.057(8) -0.006(5) -0.012(6) -0.008(5) C24 0.066(8) 0.006(4) 0.064(9) -0.001(5) 0.038(6) -0.006(4) C25 0.043(6) 0.014(4) 0.058(8) 0.011(5) 0.001(5) 0.004(4) C26 0.034(5) 0.031(5) 0.043(7) 0.005(5) 0.010(5) -0.011(4) C27 0.046(6) 0.019(5) 0.054(8) -0.007(5) -0.005(5) -0.010(4) Pt2 0.02155(15) 0.02561(15) 0.01939(17) 0.00217(14) 0.00042(18) 0.00083(12) Ru2 0.0225(4) 0.0203(3) 0.0306(4) 0.0032(3) 0.0011(3) -0.0025(3) Cl2 0.0277(12) 0.0424(14) 0.0324(14) 0.0044(11) -0.0055(10) 0.0039(10) P3 0.0258(13) 0.0279(12) 0.0176(13) 0.0004(10) 0.0021(9) -0.0005(10) P4 0.0232(12) 0.0241(12) 0.0229(13) 0.0033(10) 0.0029(9) 0.0018(9) O3 0.023(3) 0.046(4) 0.020(4) -0.003(3) 0.000(3) -0.004(3) O4 0.027(3) 0.037(3) 0.025(4) 0.002(3) 0.007(3) -0.003(3) C28 0.029(5) 0.031(5) 0.012(5) -0.004(4) 0.004(4) -0.006(4) C29 0.017(4) 0.025(4) 0.025(5) -0.003(4) 0.001(4) 0.001(4) C30 0.028(4) 0.012(4) 0.024(5) 0.000(3) 0.004(4) -0.007(3) C31 0.026(5) 0.016(4) 0.033(6) 0.002(4) 0.003(4) -0.003(3) C32 0.034(5) 0.026(5) 0.012(5) 0.003(4) 0.010(4) 0.000(4) C33 0.017(4) 0.021(4) 0.023(5) 0.008(4) -0.002(3) -0.002(3) C34 0.028(5) 0.027(5) 0.045(7) -0.006(4) 0.004(4) 0.000(4) C35 0.025(5) 0.025(5) 0.035(6) -0.002(4) -0.002(4) -0.002(4) C36 0.025(5) 0.021(5) 0.052(7) 0.006(5) -0.010(4) -0.002(4) C37 0.040(5) 0.017(4) 0.019(5) 0.006(4) 0.006(4) -0.006(4) C38 0.035(5) 0.019(4) 0.033(6) -0.001(4) 0.007(4) -0.003(4) C39 0.062(7) 0.021(5) 0.060(8) -0.007(5) 0.017(6) -0.010(5) C40 0.044(6) 0.048(7) 0.057(8) 0.007(6) 0.025(5) -0.008(5) C41 0.037(5) 0.030(5) 0.030(6) -0.004(4) -0.001(4) 0.006(4) C42 0.086(8) 0.039(6) 0.035(7) -0.004(6) -0.006(7) 0.018(5) C43 0.069(8) 0.014(5) 0.053(8) 0.005(5) -0.005(6) 0.005(5) C44 0.052(6) 0.037(5) 0.020(5) -0.005(4) 0.012(5) 0.011(5) C45 0.106(11) 0.030(6) 0.048(8) -0.004(6) -0.019(7) 0.010(6) C46 0.034(6) 0.041(6) 0.081(10) -0.001(6) 0.005(6) 0.025(5) C47 0.031(5) 0.042(6) 0.037(7) 0.007(5) -0.004(4) -0.012(4) C48 0.046(7) 0.082(10) 0.060(9) 0.018(8) 0.009(6) -0.027(7) C49 0.054(8) 0.031(6) 0.115(13) -0.011(7) 0.002(8) -0.010(6) C50 0.062(8) 0.029(6) 0.044(7) -0.017(5) 0.013(6) -0.007(5) C51 0.038(6) 0.016(5) 0.110(13) 0.009(6) 0.000(7) 0.000(4) C52 0.111(12) 0.035(6) 0.030(7) 0.018(5) -0.016(7) -0.025(7) C53 0.061(8) 0.033(6) 0.105(13) -0.008(7) 0.054(8) -0.025(6) C54 0.040(6) 0.026(5) 0.072(10) 0.001(6) -0.014(6) -0.012(5) P5 0.0267(13) 0.0324(14) 0.0405(17) -0.0006(12) 0.0023(11) 0.0013(10) F1 0.161(10) 0.125(8) 0.019(4) 0.001(5) -0.001(5) 0.045(7) F2 0.051(5) 0.049(4) 0.176(10) 0.035(6) 0.003(5) -0.023(4) F3 0.064(5) 0.070(5) 0.064(5) 0.009(4) -0.007(4) 0.034(4) F4 0.052(4) 0.080(5) 0.099(7) 0.004(5) -0.001(4) -0.032(4) F5 0.068(5) 0.042(4) 0.089(6) 0.013(4) 0.028(4) 0.029(3) F6 0.083(5) 0.068(5) 0.038(4) -0.008(4) 0.001(4) 0.020(4) P6 0.0353(15) 0.0407(16) 0.0436(19) 0.0022(13) -0.0042(12) -0.0047(12) F7 0.163(12) 0.32(2) 0.041(6) -0.004(9) -0.025(7) -0.093(12) F8 0.094(8) 0.128(9) 0.203(15) 0.044(10) 0.028(8) 0.058(7) F9 0.079(6) 0.172(11) 0.137(10) 0.106(9) -0.019(6) -0.052(7) F10 0.214(14) 0.081(7) 0.261(19) 0.024(10) 0.115(14) 0.086(9) F11 0.064(6) 0.223(14) 0.224(15) 0.159(12) -0.002(7) -0.049(7) F12 0.086(8) 0.187(12) 0.175(13) -0.068(11) -0.063(8) -0.027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 1.975(9) . ? Pt1 P2 2.266(3) . ? Pt1 P1 2.270(3) . ? Pt1 Cl1 2.376(3) . ? Ru1 C23 2.146(11) . ? Ru1 C26 2.170(9) . ? Ru1 C27 2.175(10) . ? Ru1 C25 2.182(9) . ? Ru1 C10 2.184(8) . ? Ru1 C24 2.188(9) . ? Ru1 C9 2.205(9) . ? Ru1 C8 2.206(10) . ? Ru1 C7 2.221(10) . ? Ru1 C5 2.268(9) . ? Ru1 C4 2.330(9) . ? P1 O1 1.634(7) . ? P1 C11 1.815(9) . ? P1 C14 1.827(10) . ? P2 O2 1.653(7) . ? P2 C20 1.812(10) . ? P2 C17 1.822(10) . ? O1 C2 1.387(11) . ? O2 C6 1.371(11) . ? C1 C6 1.377(13) . ? C1 C2 1.433(14) . ? C2 C3 1.362(13) . ? C3 C4 1.415(13) . ? C3 H3 0.9500 . ? C4 C7 1.429(12) . ? C4 C5 1.470(13) . ? C5 C6 1.412(12) . ? C5 C10 1.422(12) . ? C7 C8 1.419(14) . ? C7 H7 0.9500 . ? C8 C9 1.390(15) . ? C8 H8 0.9500 . ? C9 C10 1.416(13) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C13 1.472(15) . ? C11 C12 1.543(13) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.516(14) . ? C14 C16 1.529(14) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.510(15) . ? C17 C18 1.519(16) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.525(15) . ? C20 C22 1.532(14) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.391(17) . ? C23 C27 1.392(17) . ? C23 H23 0.9500 . ? C24 C25 1.444(16) . ? C24 H24 0.9500 . ? C25 C26 1.432(15) . ? C25 H25 0.9500 . ? C26 C27 1.413(16) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? Pt2 C28 1.976(10) . ? Pt2 P3 2.261(2) . ? Pt2 P4 2.268(3) . ? Pt2 Cl2 2.373(2) . ? Ru2 C53 2.154(10) . ? Ru2 C54 2.160(11) . ? Ru2 C51 2.166(10) . ? Ru2 C52 2.173(11) . ? Ru2 C34 2.175(10) . ? Ru2 C50 2.176(10) . ? Ru2 C35 2.187(9) . ? Ru2 C36 2.210(9) . ? Ru2 C37 2.213(9) . ? Ru2 C30 2.270(9) . ? Ru2 C31 2.297(9) . ? P3 O3 1.676(7) . ? P3 C41 1.815(10) . ? P3 C38 1.824(9) . ? P4 O4 1.670(7) . ? P4 C47 1.813(10) . ? P4 C44 1.823(9) . ? O3 C29 1.393(11) . ? O4 C33 1.383(10) . ? C28 C29 1.347(13) . ? C28 C33 1.438(13) . ? C29 C30 1.436(13) . ? C30 C34 1.424(12) . ? C30 C31 1.437(13) . ? C31 C37 1.426(13) . ? C31 C32 1.445(12) . ? C32 C33 1.349(13) . ? C32 H32 0.9500 . ? C34 C35 1.386(14) . ? C34 H34 0.9500 . ? C35 C36 1.414(14) . ? C35 H35 0.9500 . ? C36 C37 1.395(13) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C40 1.548(13) . ? C38 C39 1.560(14) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.533(15) . ? C41 C43 1.547(13) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.495(15) . ? C44 C45 1.511(16) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.513(16) . ? C47 C48 1.521(16) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.366(18) . ? C50 C54 1.376(17) . ? C50 H50 0.9500 . ? C51 C52 1.401(19) . ? C51 H51 0.9500 . ? C52 C53 1.39(2) . ? C52 H52 0.9500 . ? C53 C54 1.429(19) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? P5 F2 1.565(7) . ? P5 F1 1.567(8) . ? P5 F6 1.570(8) . ? P5 F4 1.580(7) . ? P5 F5 1.586(7) . ? P5 F3 1.593(7) . ? P6 F12 1.506(11) . ? P6 F10 1.518(10) . ? P6 F7 1.522(11) . ? P6 F9 1.543(9) . ? P6 F8 1.572(11) . ? P6 F11 1.572(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P2 80.8(3) . . ? C1 Pt1 P1 81.3(3) . . ? P2 Pt1 P1 161.41(9) . . ? C1 Pt1 Cl1 176.9(3) . . ? P2 Pt1 Cl1 97.25(10) . . ? P1 Pt1 Cl1 100.87(10) . . ? C23 Ru1 C26 63.4(5) . . ? C23 Ru1 C27 37.6(4) . . ? C26 Ru1 C27 38.0(4) . . ? C23 Ru1 C25 63.9(5) . . ? C26 Ru1 C25 38.4(4) . . ? C27 Ru1 C25 63.9(4) . . ? C23 Ru1 C10 105.3(4) . . ? C26 Ru1 C10 152.4(4) . . ? C27 Ru1 C10 117.6(4) . . ? C25 Ru1 C10 161.6(4) . . ? C23 Ru1 C24 37.4(5) . . ? C26 Ru1 C24 63.7(4) . . ? C27 Ru1 C24 62.9(4) . . ? C25 Ru1 C24 38.6(4) . . ? C10 Ru1 C24 123.9(4) . . ? C23 Ru1 C9 119.6(4) . . ? C26 Ru1 C9 123.4(4) . . ? C27 Ru1 C9 106.2(4) . . ? C25 Ru1 C9 160.4(4) . . ? C10 Ru1 C9 37.6(3) . . ? C24 Ru1 C9 154.3(5) . . ? C23 Ru1 C8 147.8(4) . . ? C26 Ru1 C8 107.6(4) . . ? C27 Ru1 C8 115.8(4) . . ? C25 Ru1 C8 129.7(4) . . ? C10 Ru1 C8 67.6(4) . . ? C24 Ru1 C8 168.3(4) . . ? C9 Ru1 C8 36.7(4) . . ? C23 Ru1 C7 173.8(4) . . ? C26 Ru1 C7 113.7(4) . . ? C27 Ru1 C7 143.1(4) . . ? C25 Ru1 C7 110.3(4) . . ? C10 Ru1 C7 79.7(4) . . ? C24 Ru1 C7 136.6(4) . . ? C9 Ru1 C7 66.6(4) . . ? C8 Ru1 C7 37.4(4) . . ? C23 Ru1 C5 115.0(4) . . ? C26 Ru1 C5 169.7(4) . . ? C27 Ru1 C5 146.3(4) . . ? C25 Ru1 C5 131.3(4) . . ? C10 Ru1 C5 37.2(3) . . ? C24 Ru1 C5 108.5(3) . . ? C9 Ru1 C5 66.7(3) . . ? C8 Ru1 C5 79.1(3) . . ? C7 Ru1 C5 66.7(3) . . ? C23 Ru1 C4 141.9(4) . . ? C26 Ru1 C4 137.7(4) . . ? C27 Ru1 C4 175.0(4) . . ? C25 Ru1 C4 111.1(4) . . ? C10 Ru1 C4 67.3(3) . . ? C24 Ru1 C4 113.8(4) . . ? C9 Ru1 C4 78.4(3) . . ? C8 Ru1 C4 66.6(3) . . ? C7 Ru1 C4 36.5(3) . . ? C5 Ru1 C4 37.2(3) . . ? O1 P1 C11 102.9(5) . . ? O1 P1 C14 101.3(4) . . ? C11 P1 C14 109.3(4) . . ? O1 P1 Pt1 104.5(3) . . ? C11 P1 Pt1 114.5(4) . . ? C14 P1 Pt1 121.6(4) . . ? O2 P2 C20 104.2(4) . . ? O2 P2 C17 102.4(4) . . ? C20 P2 C17 107.9(5) . . ? O2 P2 Pt1 103.0(3) . . ? C20 P2 Pt1 119.0(3) . . ? C17 P2 Pt1 117.8(4) . . ? C2 O1 P1 116.3(6) . . ? C6 O2 P2 115.9(6) . . ? C6 C1 C2 117.8(8) . . ? C6 C1 Pt1 121.6(8) . . ? C2 C1 Pt1 120.6(7) . . ? C3 C2 O1 118.8(9) . . ? C3 C2 C1 123.9(9) . . ? O1 C2 C1 117.3(8) . . ? C2 C3 C4 118.0(9) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C3 C4 C7 122.3(9) . . ? C3 C4 C5 120.8(8) . . ? C7 C4 C5 116.8(8) . . ? C3 C4 Ru1 131.7(7) . . ? C7 C4 Ru1 67.6(5) . . ? C5 C4 Ru1 69.1(5) . . ? C6 C5 C10 123.0(9) . . ? C6 C5 C4 117.0(8) . . ? C10 C5 C4 119.9(8) . . ? C6 C5 Ru1 129.0(6) . . ? C10 C5 Ru1 68.2(5) . . ? C4 C5 Ru1 73.7(5) . . ? O2 C6 C1 118.0(9) . . ? O2 C6 C5 119.5(8) . . ? C1 C6 C5 122.5(9) . . ? C8 C7 C4 122.0(10) . . ? C8 C7 Ru1 70.7(6) . . ? C4 C7 Ru1 75.9(6) . . ? C8 C7 H7 119.0 . . ? C4 C7 H7 119.0 . . ? Ru1 C7 H7 126.3 . . ? C9 C8 C7 119.7(9) . . ? C9 C8 Ru1 71.6(6) . . ? C7 C8 Ru1 71.9(6) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? Ru1 C8 H8 128.6 . . ? C8 C9 C10 121.0(10) . . ? C8 C9 Ru1 71.7(6) . . ? C10 C9 Ru1 70.4(5) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? Ru1 C9 H9 131.3 . . ? C9 C10 C5 120.1(9) . . ? C9 C10 Ru1 72.0(5) . . ? C5 C10 Ru1 74.6(5) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? Ru1 C10 H10 125.2 . . ? C13 C11 C12 109.7(9) . . ? C13 C11 P1 116.0(8) . . ? C12 C11 P1 109.4(6) . . ? C13 C11 H11 107.1 . . ? C12 C11 H11 107.1 . . ? P1 C11 H11 107.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 111.9(9) . . ? C15 C14 P1 109.3(7) . . ? C16 C14 P1 109.0(7) . . ? C15 C14 H14 108.9 . . ? C16 C14 H14 108.9 . . ? P1 C14 H14 108.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 114.1(10) . . ? C19 C17 P2 110.4(8) . . ? C18 C17 P2 108.4(8) . . ? C19 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? P2 C17 H17 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.9(9) . . ? C21 C20 P2 109.5(8) . . ? C22 C20 P2 113.7(7) . . ? C21 C20 H20 107.1 . . ? C22 C20 H20 107.1 . . ? P2 C20 H20 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C27 109.7(12) . . ? C24 C23 Ru1 72.9(6) . . ? C27 C23 Ru1 72.4(6) . . ? C24 C23 H23 125.1 . . ? C27 C23 H23 125.1 . . ? Ru1 C23 H23 121.2 . . ? C23 C24 C25 107.8(10) . . ? C23 C24 Ru1 69.6(6) . . ? C25 C24 Ru1 70.5(5) . . ? C23 C24 H24 126.1 . . ? C25 C24 H24 126.1 . . ? Ru1 C24 H24 125.4 . . ? C26 C25 C24 106.2(10) . . ? C26 C25 Ru1 70.3(5) . . ? C24 C25 Ru1 70.9(5) . . ? C26 C25 H25 126.9 . . ? C24 C25 H25 126.9 . . ? Ru1 C25 H25 123.5 . . ? C27 C26 C25 108.2(10) . . ? C27 C26 Ru1 71.2(6) . . ? C25 C26 Ru1 71.3(5) . . ? C27 C26 H26 125.9 . . ? C25 C26 H26 125.9 . . ? Ru1 C26 H26 123.3 . . ? C23 C27 C26 107.9(10) . . ? C23 C27 Ru1 70.1(6) . . ? C26 C27 Ru1 70.8(6) . . ? C23 C27 H27 126.0 . . ? C26 C27 H27 126.0 . . ? Ru1 C27 H27 124.7 . . ? C28 Pt2 P3 80.7(3) . . ? C28 Pt2 P4 81.0(3) . . ? P3 Pt2 P4 161.67(9) . . ? C28 Pt2 Cl2 177.2(3) . . ? P3 Pt2 Cl2 98.72(9) . . ? P4 Pt2 Cl2 99.61(9) . . ? C53 Ru2 C54 38.7(5) . . ? C53 Ru2 C51 63.1(5) . . ? C54 Ru2 C51 62.4(5) . . ? C53 Ru2 C52 37.6(5) . . ? C54 Ru2 C52 63.1(5) . . ? C51 Ru2 C52 37.7(5) . . ? C53 Ru2 C34 113.4(5) . . ? C54 Ru2 C34 145.8(4) . . ? C51 Ru2 C34 132.4(5) . . ? C52 Ru2 C34 108.3(4) . . ? C53 Ru2 C50 62.9(5) . . ? C54 Ru2 C50 37.0(5) . . ? C51 Ru2 C50 36.7(5) . . ? C52 Ru2 C50 62.1(5) . . ? C34 Ru2 C50 169.0(5) . . ? C53 Ru2 C35 107.3(4) . . ? C54 Ru2 C35 119.1(4) . . ? C51 Ru2 C35 164.1(5) . . ? C52 Ru2 C35 127.1(5) . . ? C34 Ru2 C35 37.1(4) . . ? C50 Ru2 C35 152.7(4) . . ? C53 Ru2 C36 122.8(5) . . ? C54 Ru2 C36 107.8(4) . . ? C51 Ru2 C36 158.1(5) . . ? C52 Ru2 C36 158.3(5) . . ? C34 Ru2 C36 67.2(4) . . ? C50 Ru2 C36 123.7(5) . . ? C35 Ru2 C36 37.5(4) . . ? C53 Ru2 C37 151.6(6) . . ? C54 Ru2 C37 117.6(4) . . ? C51 Ru2 C37 127.5(4) . . ? C52 Ru2 C37 164.7(5) . . ? C34 Ru2 C37 79.7(4) . . ? C50 Ru2 C37 108.4(4) . . ? C35 Ru2 C37 67.2(3) . . ? C36 Ru2 C37 36.8(4) . . ? C53 Ru2 C30 138.7(5) . . ? C54 Ru2 C30 173.6(4) . . ? C51 Ru2 C30 111.4(4) . . ? C52 Ru2 C30 111.4(4) . . ? C34 Ru2 C30 37.3(3) . . ? C50 Ru2 C30 138.4(4) . . ? C35 Ru2 C30 66.5(3) . . ? C36 Ru2 C30 78.5(3) . . ? C37 Ru2 C30 66.7(3) . . ? C53 Ru2 C31 171.1(5) . . ? C54 Ru2 C31 144.6(5) . . ? C51 Ru2 C31 109.8(4) . . ? C52 Ru2 C31 133.6(5) . . ? C34 Ru2 C31 66.8(4) . . ? C50 Ru2 C31 115.1(4) . . ? C35 Ru2 C31 78.3(3) . . ? C36 Ru2 C31 65.8(3) . . ? C37 Ru2 C31 36.8(3) . . ? C30 Ru2 C31 36.7(3) . . ? O3 P3 C41 100.2(4) . . ? O3 P3 C38 102.3(4) . . ? C41 P3 C38 108.0(5) . . ? O3 P3 Pt2 104.7(3) . . ? C41 P3 Pt2 120.4(4) . . ? C38 P3 Pt2 117.8(3) . . ? O4 P4 C47 101.5(4) . . ? O4 P4 C44 102.6(4) . . ? C47 P4 C44 109.1(5) . . ? O4 P4 Pt2 104.4(2) . . ? C47 P4 Pt2 117.5(4) . . ? C44 P4 Pt2 119.0(3) . . ? C29 O3 P3 112.0(6) . . ? C33 O4 P4 116.1(6) . . ? C29 C28 C33 116.7(9) . . ? C29 C28 Pt2 121.2(7) . . ? C33 C28 Pt2 122.1(6) . . ? C28 C29 O3 121.4(9) . . ? C28 C29 C30 124.0(9) . . ? O3 C29 C30 114.6(8) . . ? C34 C30 C29 124.5(9) . . ? C34 C30 C31 118.7(9) . . ? C29 C30 C31 116.7(8) . . ? C34 C30 Ru2 67.7(5) . . ? C29 C30 Ru2 128.2(6) . . ? C31 C30 Ru2 72.7(5) . . ? C37 C31 C30 118.9(8) . . ? C37 C31 C32 121.0(9) . . ? C30 C31 C32 120.0(8) . . ? C37 C31 Ru2 68.4(5) . . ? C30 C31 Ru2 70.7(5) . . ? C32 C31 Ru2 132.5(6) . . ? C33 C32 C31 118.0(9) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 O4 119.2(8) . . ? C32 C33 C28 124.4(8) . . ? O4 C33 C28 116.4(8) . . ? C35 C34 C30 121.0(10) . . ? C35 C34 Ru2 72.0(6) . . ? C30 C34 Ru2 75.0(5) . . ? C35 C34 H34 119.5 . . ? C30 C34 H34 119.5 . . ? Ru2 C34 H34 125.3 . . ? C34 C35 C36 120.3(9) . . ? C34 C35 Ru2 71.0(6) . . ? C36 C35 Ru2 72.1(6) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? Ru2 C35 H35 129.4 . . ? C37 C36 C35 120.1(9) . . ? C37 C36 Ru2 71.7(5) . . ? C35 C36 Ru2 70.4(6) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? Ru2 C36 H36 130.6 . . ? C36 C37 C31 120.5(9) . . ? C36 C37 Ru2 71.5(5) . . ? C31 C37 Ru2 74.8(5) . . ? C36 C37 H37 119.7 . . ? C31 C37 H37 119.7 . . ? Ru2 C37 H37 125.7 . . ? C40 C38 C39 111.3(8) . . ? C40 C38 P3 112.9(7) . . ? C39 C38 P3 108.8(7) . . ? C40 C38 H38 107.9 . . ? C39 C38 H38 107.9 . . ? P3 C38 H38 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 110.7(9) . . ? C42 C41 P3 109.2(7) . . ? C43 C41 P3 108.7(7) . . ? C42 C41 H41 109.4 . . ? C43 C41 H41 109.4 . . ? P3 C41 H41 109.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C45 112.6(9) . . ? C46 C44 P4 111.5(8) . . ? C45 C44 P4 108.3(7) . . ? C46 C44 H44 108.1 . . ? C45 C44 H44 108.1 . . ? P4 C44 H44 108.1 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C48 111.7(11) . . ? C49 C47 P4 109.5(7) . . ? C48 C47 P4 113.9(8) . . ? C49 C47 H47 107.1 . . ? C48 C47 H47 107.1 . . ? P4 C47 H47 107.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C54 109.5(12) . . ? C51 C50 Ru2 71.2(7) . . ? C54 C50 Ru2 70.8(6) . . ? C51 C50 H50 125.2 . . ? C54 C50 H50 125.2 . . ? Ru2 C50 H50 124.3 . . ? C50 C51 C52 108.3(11) . . ? C50 C51 Ru2 72.1(6) . . ? C52 C51 Ru2 71.4(7) . . ? C50 C51 H51 125.9 . . ? C52 C51 H51 125.9 . . ? Ru2 C51 H51 122.3 . . ? C53 C52 C51 108.0(12) . . ? C53 C52 Ru2 70.5(7) . . ? C51 C52 Ru2 70.9(6) . . ? C53 C52 H52 126.0 . . ? C51 C52 H52 126.0 . . ? Ru2 C52 H52 124.3 . . ? C52 C53 C54 106.8(11) . . ? C52 C53 Ru2 72.0(6) . . ? C54 C53 Ru2 70.9(6) . . ? C52 C53 H53 126.6 . . ? C54 C53 H53 126.6 . . ? Ru2 C53 H53 122.3 . . ? C50 C54 C53 107.4(12) . . ? C50 C54 Ru2 72.2(6) . . ? C53 C54 Ru2 70.4(7) . . ? C50 C54 H54 126.3 . . ? C53 C54 H54 126.3 . . ? Ru2 C54 H54 122.8 . . ? F2 P5 F1 92.2(7) . . ? F2 P5 F6 90.8(6) . . ? F1 P5 F6 177.0(6) . . ? F2 P5 F4 177.8(6) . . ? F1 P5 F4 89.7(6) . . ? F6 P5 F4 87.3(5) . . ? F2 P5 F5 90.2(4) . . ? F1 P5 F5 90.6(5) . . ? F6 P5 F5 90.1(4) . . ? F4 P5 F5 88.8(4) . . ? F2 P5 F3 89.6(4) . . ? F1 P5 F3 91.4(5) . . ? F6 P5 F3 87.9(4) . . ? F4 P5 F3 91.4(5) . . ? F5 P5 F3 178.0(5) . . ? F12 P6 F10 83.6(9) . . ? F12 P6 F7 172.3(9) . . ? F10 P6 F7 104.0(10) . . ? F12 P6 F9 90.9(7) . . ? F10 P6 F9 89.6(7) . . ? F7 P6 F9 90.6(7) . . ? F12 P6 F8 89.0(8) . . ? F10 P6 F8 172.4(9) . . ? F7 P6 F8 83.4(9) . . ? F9 P6 F8 88.7(7) . . ? F12 P6 F11 92.3(8) . . ? F10 P6 F11 88.8(8) . . ? F7 P6 F11 86.5(7) . . ? F9 P6 F11 176.2(9) . . ? F8 P6 F11 93.2(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.417 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.168 #============================================================================== data_compound-5a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl Fe Ni O2 P2, F6 P' _chemical_formula_sum 'C27 H38 Cl F6 Fe Ni O2 P3' _chemical_formula_weight 751.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.0269(14) _cell_length_b 13.2282(11) _cell_length_c 28.684(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6460.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8557 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 21.56 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6463 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector 01-670' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 67751 _diffrn_reflns_av_R_equivalents 0.1218 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.45 _reflns_number_total 5930 _reflns_number_gt 3192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _publ_section_exptl_refinement ;The isopropyl fragments and PF~6~ are disordered and were modelled in two major contributors, using a free variable for site occupational factor (SOF). The ratio of SOF for isopropyl gruops was 0.42/0.58, 0.63/0.37, 0.70/0.30, 0.80/0.20 and for PF~6~ anion was 0.63/0.37, respectively. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5930 _refine_ls_number_parameters 495 _refine_ls_number_restraints 703 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.32545(7) 0.69706(9) 0.09341(4) 0.0578(4) Uani 1 1 d . . . Ni Ni 0.02226(6) 0.64899(8) 0.18156(3) 0.0551(3) Uani 1 1 d . . . Cl Cl -0.07576(15) 0.6674(2) 0.22980(9) 0.0939(9) Uani 1 1 d . . . P1 P 0.11349(13) 0.65067(18) 0.23362(8) 0.0598(6) Uani 1 1 d . A . P2 P -0.04365(13) 0.64838(19) 0.11670(8) 0.0635(6) Uani 1 1 d . B . O1 O 0.1967(3) 0.6300(4) 0.20422(19) 0.0659(16) Uani 1 1 d . . . O2 O 0.0203(3) 0.6213(5) 0.0762(2) 0.0821(19) Uani 1 1 d . . . C1 C 0.1798(5) 0.6177(5) 0.1572(3) 0.054(2) Uani 1 1 d . . . C2 C 0.1062(4) 0.6267(5) 0.1406(3) 0.0482(19) Uani 1 1 d . . . C3 C 0.0954(4) 0.6173(6) 0.0915(3) 0.0492(19) Uani 1 1 d . . . C4 C 0.1545(5) 0.6021(7) 0.0615(3) 0.064(2) Uani 1 1 d . . . H4 H 0.1452 0.5999 0.0296 0.077 Uiso 1 1 calc R . . C5 C 0.2986(6) 0.5793(7) 0.0484(3) 0.078(3) Uani 1 1 d . . . H5 H 0.2907 0.5819 0.0163 0.094 Uiso 1 1 calc R . . C6 C 0.3738(6) 0.5657(7) 0.0656(5) 0.085(3) Uani 1 1 d . . . H6 H 0.4155 0.5540 0.0453 0.102 Uiso 1 1 calc R . . C7 C 0.3866(5) 0.5699(7) 0.1140(4) 0.083(3) Uani 1 1 d . . . H7 H 0.4372 0.5610 0.1253 0.100 Uiso 1 1 calc R . . C8 C 0.3250(5) 0.5872(6) 0.1457(3) 0.070(2) Uani 1 1 d . . . H8 H 0.3347 0.5930 0.1775 0.084 Uiso 1 1 calc R . . C9 C 0.2480(5) 0.5954(6) 0.1278(3) 0.055(2) Uani 1 1 d . . . C10 C 0.2322(5) 0.5893(5) 0.0794(3) 0.054(2) Uani 1 1 d . . . C11 C 0.3246(8) 0.8270(8) 0.1303(5) 0.111(3) Uani 1 1 d . . . H11 H 0.3137 0.8323 0.1620 0.133 Uiso 1 1 calc R . . C12 C 0.2707(9) 0.8336(8) 0.0969(5) 0.111(3) Uani 1 1 d . . . H12 H 0.2171 0.8431 0.1014 0.133 Uiso 1 1 calc R . . C13 C 0.3083(7) 0.8240(7) 0.0544(5) 0.100(4) Uani 1 1 d . . . H13 H 0.2852 0.8256 0.0250 0.120 Uiso 1 1 calc R . . C14 C 0.3884(6) 0.8112(7) 0.0645(5) 0.092(3) Uani 1 1 d . . . H14 H 0.4287 0.8037 0.0429 0.110 Uiso 1 1 calc R . . C15 C 0.3966(8) 0.8116(8) 0.1126(6) 0.109(4) Uani 1 1 d . . . H15 H 0.4429 0.8029 0.1294 0.131 Uiso 1 1 calc R . . C16 C 0.1182(6) 0.5503(7) 0.2768(3) 0.085(3) Uani 1 1 d DU . . H16 H 0.0779 0.5690 0.2996 0.102 Uiso 0.413(13) 1 calc PR A 1 H16A H 0.1678 0.5574 0.2939 0.102 Uiso 0.587(13) 1 calc PR A 2 C17 C 0.0903(17) 0.4521(17) 0.2579(13) 0.100(7) Uani 0.413(13) 1 d PDU A 1 H17A H 0.0414 0.4620 0.2418 0.150 Uiso 0.413(13) 1 calc PR A 1 H17B H 0.0828 0.4052 0.2831 0.150 Uiso 0.413(13) 1 calc PR A 1 H17C H 0.1286 0.4256 0.2366 0.150 Uiso 0.413(13) 1 calc PR A 1 C18 C 0.1913(10) 0.544(2) 0.3048(8) 0.104(7) Uani 0.413(13) 1 d PDU A 1 H18A H 0.2056 0.6105 0.3153 0.157 Uiso 0.413(13) 1 calc PR A 1 H18B H 0.2328 0.5168 0.2860 0.157 Uiso 0.413(13) 1 calc PR A 1 H18C H 0.1826 0.5011 0.3313 0.157 Uiso 0.413(13) 1 calc PR A 1 C17A C 0.1214(14) 0.4539(13) 0.2501(9) 0.101(6) Uani 0.587(13) 1 d PDU A 2 H17D H 0.1661 0.4547 0.2297 0.152 Uiso 0.587(13) 1 calc PR A 2 H17E H 0.0743 0.4467 0.2320 0.152 Uiso 0.587(13) 1 calc PR A 2 H17F H 0.1258 0.3982 0.2714 0.152 Uiso 0.587(13) 1 calc PR A 2 C18A C 0.0535(9) 0.5587(14) 0.3105(5) 0.108(6) Uani 0.587(13) 1 d PDU A 2 H18D H 0.0590 0.6202 0.3279 0.161 Uiso 0.587(13) 1 calc PR A 2 H18E H 0.0549 0.5021 0.3314 0.161 Uiso 0.587(13) 1 calc PR A 2 H18F H 0.0043 0.5593 0.2941 0.161 Uiso 0.587(13) 1 calc PR A 2 C19 C 0.1326(6) 0.7719(7) 0.2624(3) 0.085(3) Uani 1 1 d DU . . H19 H 0.0879 0.7843 0.2831 0.102 Uiso 0.633(14) 1 calc PR A 1 H19A H 0.1848 0.7650 0.2764 0.102 Uiso 0.367(14) 1 calc PR A 2 C20 C 0.2034(8) 0.7724(13) 0.2922(6) 0.106(5) Uani 0.633(14) 1 d PDU A 1 H20A H 0.2013 0.7163 0.3135 0.158 Uiso 0.633(14) 1 calc PR A 1 H20B H 0.2055 0.8344 0.3096 0.158 Uiso 0.633(14) 1 calc PR A 1 H20C H 0.2494 0.7667 0.2731 0.158 Uiso 0.633(14) 1 calc PR A 1 C21 C 0.130(2) 0.852(2) 0.2259(10) 0.105(6) Uani 0.633(14) 1 d PDU A 1 H21A H 0.0816 0.8466 0.2088 0.158 Uiso 0.633(14) 1 calc PR A 1 H21B H 0.1734 0.8441 0.2051 0.158 Uiso 0.633(14) 1 calc PR A 1 H21C H 0.1326 0.9174 0.2405 0.158 Uiso 0.633(14) 1 calc PR A 1 C20A C 0.0782(15) 0.786(2) 0.3021(8) 0.109(8) Uani 0.367(14) 1 d PDU A 2 H20D H 0.0876 0.7348 0.3250 0.163 Uiso 0.367(14) 1 calc PR A 2 H20E H 0.0250 0.7816 0.2912 0.163 Uiso 0.367(14) 1 calc PR A 2 H20F H 0.0868 0.8516 0.3157 0.163 Uiso 0.367(14) 1 calc PR A 2 C21A C 0.139(4) 0.859(3) 0.2299(17) 0.103(7) Uani 0.367(14) 1 d PDU A 2 H21D H 0.1772 0.8443 0.2063 0.154 Uiso 0.367(14) 1 calc PR A 2 H21E H 0.1546 0.9182 0.2469 0.154 Uiso 0.367(14) 1 calc PR A 2 H21F H 0.0888 0.8709 0.2155 0.154 Uiso 0.367(14) 1 calc PR A 2 C22 C -0.1167(6) 0.5496(8) 0.1076(3) 0.090(3) Uani 1 1 d DU . . H22 H -0.1643 0.5718 0.1239 0.108 Uiso 0.709(11) 1 calc PR B 1 H22A H -0.1417 0.5706 0.0784 0.108 Uiso 0.291(11) 1 calc PR B 2 C23 C -0.1406(8) 0.5285(11) 0.0584(4) 0.100(5) Uani 0.709(11) 1 d PDU B 1 H23A H -0.1547 0.5907 0.0433 0.150 Uiso 0.709(11) 1 calc PR B 1 H23B H -0.1848 0.4835 0.0582 0.150 Uiso 0.709(11) 1 calc PR B 1 H23C H -0.0976 0.4978 0.0420 0.150 Uiso 0.709(11) 1 calc PR B 1 C24 C -0.0896(11) 0.4566(10) 0.1320(6) 0.122(5) Uani 0.709(11) 1 d PDU B 1 H24A H -0.0759 0.4728 0.1636 0.183 Uiso 0.709(11) 1 calc PR B 1 H24B H -0.0446 0.4296 0.1162 0.183 Uiso 0.709(11) 1 calc PR B 1 H24C H -0.1310 0.4073 0.1319 0.183 Uiso 0.709(11) 1 calc PR B 1 C23A C -0.083(2) 0.4506(17) 0.0952(15) 0.123(7) Uani 0.291(11) 1 d PDU B 2 H23D H -0.0424 0.4599 0.0721 0.184 Uiso 0.291(11) 1 calc PR B 2 H23E H -0.1230 0.4076 0.0828 0.184 Uiso 0.291(11) 1 calc PR B 2 H23F H -0.0604 0.4198 0.1224 0.184 Uiso 0.291(11) 1 calc PR B 2 C24A C -0.1834(12) 0.549(2) 0.1406(9) 0.090(8) Uani 0.291(11) 1 d PDU B 2 H24D H -0.2099 0.6125 0.1395 0.135 Uiso 0.291(11) 1 calc PR B 2 H24E H -0.1642 0.5367 0.1716 0.135 Uiso 0.291(11) 1 calc PR B 2 H24F H -0.2193 0.4957 0.1321 0.135 Uiso 0.291(11) 1 calc PR B 2 C25 C -0.0803(6) 0.7657(7) 0.0945(4) 0.106(3) Uani 1 1 d DU . . H25 H -0.0969 0.7519 0.0624 0.128 Uiso 0.805(14) 1 calc PR B 1 H25A H -0.1210 0.7719 0.1185 0.128 Uiso 0.195(14) 1 calc PR B 2 C26 C -0.0170(9) 0.8430(11) 0.0910(6) 0.126(5) Uani 0.805(14) 1 d PDU B 1 H26A H 0.0264 0.8157 0.0737 0.189 Uiso 0.805(14) 1 calc PR B 1 H26B H 0.0003 0.8613 0.1217 0.189 Uiso 0.805(14) 1 calc PR B 1 H26C H -0.0368 0.9018 0.0753 0.189 Uiso 0.805(14) 1 calc PR B 1 C27 C -0.1518(7) 0.7983(11) 0.1195(6) 0.120(5) Uani 0.805(14) 1 d PDU B 1 H27A H -0.1906 0.7458 0.1179 0.180 Uiso 0.805(14) 1 calc PR B 1 H27B H -0.1721 0.8586 0.1053 0.180 Uiso 0.805(14) 1 calc PR B 1 H27C H -0.1392 0.8117 0.1515 0.180 Uiso 0.805(14) 1 calc PR B 1 C26A C -0.029(4) 0.843(3) 0.116(2) 0.115(8) Uani 0.195(14) 1 d PDU B 2 H26D H 0.0015 0.8130 0.1407 0.173 Uiso 0.195(14) 1 calc PR B 2 H26E H -0.0602 0.8969 0.1286 0.173 Uiso 0.195(14) 1 calc PR B 2 H26F H 0.0063 0.8702 0.0929 0.173 Uiso 0.195(14) 1 calc PR B 2 C27A C -0.131(3) 0.804(4) 0.0568(14) 0.107(10) Uani 0.195(14) 1 d PDU B 2 H27D H -0.1829 0.7749 0.0598 0.161 Uiso 0.195(14) 1 calc PR B 2 H27E H -0.1096 0.7857 0.0271 0.161 Uiso 0.195(14) 1 calc PR B 2 H27F H -0.1352 0.8763 0.0589 0.161 Uiso 0.195(14) 1 calc PR B 2 P3 P 0.61947(16) 0.6625(2) 0.04842(11) 0.0891(8) Uani 1 1 d DU . . F1 F 0.6728(7) 0.5849(9) 0.0714(5) 0.185(4) Uani 0.628(7) 1 d PDU C 1 F2 F 0.5574(6) 0.5800(7) 0.0382(5) 0.160(4) Uani 0.628(7) 1 d PDU C 1 F3 F 0.5801(8) 0.6878(10) 0.0949(3) 0.161(4) Uani 0.628(7) 1 d PDU C 1 F4 F 0.5667(6) 0.7420(8) 0.0244(4) 0.142(3) Uani 0.628(7) 1 d PDU C 1 F5 F 0.6814(6) 0.7450(8) 0.0543(5) 0.162(4) Uani 0.628(7) 1 d PDU C 1 F6 F 0.6517(7) 0.6382(8) -0.0009(3) 0.141(3) Uani 0.628(7) 1 d PDU C 1 F1A F 0.5683(10) 0.7573(10) 0.0540(7) 0.153(5) Uani 0.372(7) 1 d PDU C 2 F2A F 0.6780(9) 0.7271(13) 0.0207(6) 0.154(5) Uani 0.372(7) 1 d PDU C 2 F3A F 0.5740(11) 0.6334(14) 0.0046(5) 0.157(4) Uani 0.372(7) 1 d PDU C 2 F4A F 0.6721(10) 0.5698(10) 0.0408(7) 0.150(5) Uani 0.372(7) 1 d PDU C 2 F5A F 0.5622(9) 0.6017(13) 0.0788(6) 0.148(5) Uani 0.372(7) 1 d PDU C 2 F6A F 0.6650(9) 0.6904(13) 0.0931(4) 0.136(4) Uani 0.372(7) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0457(7) 0.0498(7) 0.0778(9) -0.0041(6) 0.0079(6) -0.0044(6) Ni 0.0510(6) 0.0594(6) 0.0548(6) -0.0040(5) 0.0092(5) -0.0037(5) Cl 0.0716(16) 0.120(2) 0.0896(19) -0.0075(16) 0.0293(14) 0.0040(15) P1 0.0596(14) 0.0674(15) 0.0523(13) -0.0017(12) 0.0048(10) -0.0042(11) P2 0.0540(13) 0.0731(16) 0.0634(14) 0.0011(13) -0.0014(11) -0.0041(12) O1 0.051(3) 0.091(5) 0.056(3) 0.005(3) 0.001(3) -0.001(3) O2 0.053(4) 0.129(6) 0.064(4) 0.001(4) -0.007(3) -0.012(4) C1 0.066(6) 0.043(4) 0.053(5) 0.001(4) 0.001(4) -0.003(4) C2 0.053(5) 0.040(4) 0.051(5) 0.003(4) 0.010(4) -0.005(3) C3 0.047(5) 0.057(5) 0.043(5) -0.004(4) 0.003(4) -0.007(4) C4 0.070(6) 0.078(6) 0.045(5) -0.005(4) -0.005(4) -0.023(5) C5 0.082(7) 0.073(6) 0.081(7) -0.028(5) 0.027(6) -0.011(5) C6 0.061(6) 0.069(6) 0.125(10) -0.010(7) 0.026(6) 0.005(5) C7 0.062(6) 0.075(7) 0.112(9) 0.011(6) 0.022(6) 0.027(5) C8 0.062(6) 0.074(6) 0.073(6) 0.013(5) 0.001(5) 0.021(5) C9 0.055(5) 0.044(4) 0.067(5) -0.001(4) 0.010(5) 0.000(4) C10 0.061(5) 0.040(5) 0.061(5) -0.004(4) 0.009(4) -0.008(4) C11 0.121(10) 0.059(5) 0.153(11) -0.026(6) 0.031(7) -0.013(6) C12 0.121(10) 0.059(5) 0.153(11) -0.026(6) 0.031(7) -0.013(6) C13 0.111(10) 0.061(7) 0.128(10) 0.028(6) -0.038(8) -0.009(6) C14 0.054(6) 0.070(7) 0.152(12) 0.020(7) 0.026(7) -0.016(5) C15 0.101(10) 0.077(8) 0.149(12) 0.011(8) -0.043(9) -0.041(7) C16 0.092(7) 0.097(6) 0.065(6) 0.020(5) -0.002(4) -0.006(6) C17 0.106(16) 0.091(10) 0.104(14) 0.034(10) 0.003(13) -0.024(12) C18 0.110(14) 0.120(16) 0.084(15) 0.020(12) -0.020(10) 0.007(12) C17A 0.114(14) 0.082(9) 0.108(12) 0.023(8) 0.017(11) -0.007(10) C18A 0.130(13) 0.133(13) 0.060(10) 0.027(9) 0.015(8) -0.008(11) C19 0.094(6) 0.078(6) 0.083(7) -0.023(4) -0.006(5) -0.011(5) C20 0.098(11) 0.103(12) 0.116(12) -0.030(9) -0.018(8) -0.017(9) C21 0.135(12) 0.066(9) 0.115(11) -0.012(7) -0.002(9) -0.014(10) C20A 0.119(17) 0.108(17) 0.099(15) -0.031(12) 0.010(11) -0.005(15) C21A 0.131(15) 0.065(11) 0.113(13) -0.020(9) 0.003(12) -0.015(12) C22 0.075(6) 0.111(7) 0.084(6) -0.017(5) -0.006(5) -0.024(6) C23 0.095(10) 0.118(11) 0.088(8) -0.016(8) -0.016(8) -0.045(9) C24 0.145(12) 0.117(10) 0.104(11) -0.001(8) -0.018(10) -0.032(9) C23A 0.136(15) 0.118(12) 0.114(16) -0.023(14) -0.012(14) -0.006(12) C24A 0.075(15) 0.124(18) 0.071(16) 0.007(14) -0.008(10) -0.043(13) C25 0.100(7) 0.078(7) 0.140(9) 0.024(6) -0.006(6) 0.006(5) C26 0.137(10) 0.081(8) 0.159(13) 0.046(9) 0.016(10) -0.010(7) C27 0.103(9) 0.102(10) 0.156(13) -0.004(9) -0.009(8) 0.018(8) C26A 0.122(16) 0.077(14) 0.146(18) 0.036(15) -0.014(14) -0.008(12) C27A 0.10(2) 0.08(2) 0.14(2) 0.019(16) -0.003(14) 0.015(16) P3 0.0683(17) 0.094(2) 0.105(2) -0.0005(16) 0.0169(14) 0.0035(13) F1 0.162(7) 0.177(7) 0.216(9) 0.036(8) -0.007(7) 0.069(6) F2 0.150(7) 0.161(7) 0.170(9) 0.005(7) 0.027(6) -0.073(6) F3 0.169(8) 0.211(9) 0.105(5) -0.005(5) 0.035(6) 0.033(7) F4 0.147(7) 0.152(7) 0.126(7) 0.014(6) 0.000(6) 0.050(5) F5 0.146(7) 0.163(7) 0.177(10) -0.035(7) -0.007(7) -0.057(5) F6 0.127(7) 0.155(8) 0.142(5) -0.041(5) 0.057(5) -0.018(6) F1A 0.154(9) 0.146(7) 0.160(11) -0.008(7) 0.022(8) 0.061(7) F2A 0.152(9) 0.171(9) 0.140(9) 0.015(9) 0.060(8) -0.034(7) F3A 0.164(9) 0.179(10) 0.129(7) -0.018(7) -0.025(7) -0.003(8) F4A 0.160(9) 0.144(7) 0.146(11) -0.016(7) 0.029(8) 0.062(7) F5A 0.126(8) 0.165(10) 0.152(9) 0.007(9) 0.049(7) -0.043(7) F6A 0.124(9) 0.168(10) 0.115(7) -0.013(7) -0.004(6) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C15 2.017(10) . ? Fe C11 2.019(11) . ? Fe C14 2.029(9) . ? Fe C12 2.036(12) . ? Fe C13 2.039(10) . ? Fe C7 2.064(9) . ? Fe C5 2.075(9) . ? Fe C6 2.082(10) . ? Fe C8 2.088(9) . ? Fe C9 2.126(8) . ? Fe C10 2.171(8) . ? Ni C2 1.873(7) . ? Ni P1 2.155(2) . ? Ni P2 2.173(3) . ? Ni Cl 2.182(2) . ? P1 O1 1.672(6) . ? P1 C16 1.817(9) . ? P1 C19 1.833(9) . ? P2 O2 1.632(6) . ? P2 C25 1.790(10) . ? P2 C22 1.823(9) . ? O1 C1 1.388(9) . ? O2 C3 1.353(8) . ? C1 C2 1.346(10) . ? C1 C9 1.465(10) . ? C2 C3 1.427(10) . ? C3 C4 1.339(10) . ? C4 C10 1.427(11) . ? C5 C6 1.383(13) . ? C5 C10 1.445(11) . ? C6 C7 1.406(14) . ? C7 C8 1.407(11) . ? C8 C9 1.411(10) . ? C9 C10 1.418(11) . ? C11 C12 1.330(16) . ? C11 C15 1.343(16) . ? C12 C13 1.384(15) . ? C13 C14 1.405(14) . ? C14 C15 1.387(16) . ? C16 C18A 1.471(9) . ? C16 C18 1.484(9) . ? C16 C17 1.485(9) . ? C16 C17A 1.488(9) . ? C19 C20 1.478(8) . ? C19 C20A 1.479(9) . ? C19 C21A 1.486(9) . ? C19 C21 1.491(9) . ? C22 C23A 1.476(9) . ? C22 C24A 1.477(9) . ? C22 C24 1.488(9) . ? C22 C23 1.497(8) . ? C25 C27 1.477(8) . ? C25 C27A 1.478(9) . ? C25 C26A 1.488(10) . ? C25 C26 1.489(8) . ? P3 F1 1.521(7) . ? P3 F3A 1.525(7) . ? P3 F5 1.526(6) . ? P3 F3 1.528(6) . ? P3 F5A 1.534(7) . ? P3 F4A 1.535(7) . ? P3 F2A 1.535(7) . ? P3 F1A 1.536(7) . ? P3 F6A 1.543(7) . ? P3 F4 1.546(6) . ? P3 F2 1.547(6) . ? P3 F6 1.550(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Fe C11 38.9(5) . . ? C15 Fe C14 40.1(5) . . ? C11 Fe C14 65.5(5) . . ? C15 Fe C12 66.1(5) . . ? C11 Fe C12 38.3(4) . . ? C14 Fe C12 66.6(5) . . ? C15 Fe C13 67.5(5) . . ? C11 Fe C13 65.5(5) . . ? C14 Fe C13 40.4(4) . . ? C12 Fe C13 39.7(4) . . ? C15 Fe C7 103.4(5) . . ? C11 Fe C7 123.2(6) . . ? C14 Fe C7 117.2(4) . . ? C12 Fe C7 160.1(5) . . ? C13 Fe C7 154.2(5) . . ? C15 Fe C5 150.1(5) . . ? C11 Fe C5 164.6(5) . . ? C14 Fe C5 114.9(5) . . ? C12 Fe C5 126.6(5) . . ? C13 Fe C5 104.2(5) . . ? C7 Fe C5 71.1(4) . . ? C15 Fe C6 119.6(5) . . ? C11 Fe C6 156.2(5) . . ? C14 Fe C6 104.8(4) . . ? C12 Fe C6 160.2(6) . . ? C13 Fe C6 122.2(5) . . ? C7 Fe C6 39.7(4) . . ? C5 Fe C6 38.9(4) . . ? C15 Fe C8 109.2(5) . . ? C11 Fe C8 102.5(5) . . ? C14 Fe C8 144.4(5) . . ? C12 Fe C8 125.5(5) . . ? C13 Fe C8 165.2(5) . . ? C7 Fe C8 39.6(3) . . ? C5 Fe C8 85.6(4) . . ? C6 Fe C8 72.3(4) . . ? C15 Fe C9 136.1(5) . . ? C11 Fe C9 106.9(4) . . ? C14 Fe C9 171.1(4) . . ? C12 Fe C9 104.7(4) . . ? C13 Fe C9 133.4(4) . . ? C7 Fe C9 70.4(3) . . ? C5 Fe C9 71.2(3) . . ? C6 Fe C9 84.0(3) . . ? C8 Fe C9 39.1(3) . . ? C15 Fe C10 169.4(5) . . ? C11 Fe C10 130.6(4) . . ? C14 Fe C10 143.1(5) . . ? C12 Fe C10 104.9(5) . . ? C13 Fe C10 109.5(4) . . ? C7 Fe C10 83.5(4) . . ? C5 Fe C10 39.7(3) . . ? C6 Fe C10 70.8(3) . . ? C8 Fe C10 71.0(3) . . ? C9 Fe C10 38.5(3) . . ? C2 Ni P1 83.5(3) . . ? C2 Ni P2 81.8(3) . . ? P1 Ni P2 164.97(10) . . ? C2 Ni Cl 177.3(2) . . ? P1 Ni Cl 96.36(10) . . ? P2 Ni Cl 98.53(10) . . ? O1 P1 C16 100.7(4) . . ? O1 P1 C19 102.7(4) . . ? C16 P1 C19 108.9(4) . . ? O1 P1 Ni 105.1(2) . . ? C16 P1 Ni 119.8(3) . . ? C19 P1 Ni 116.7(3) . . ? O2 P2 C25 99.8(4) . . ? O2 P2 C22 101.3(4) . . ? C25 P2 C22 109.4(5) . . ? O2 P2 Ni 105.4(2) . . ? C25 P2 Ni 118.8(4) . . ? C22 P2 Ni 118.5(3) . . ? C1 O1 P1 109.5(5) . . ? C3 O2 P2 114.1(5) . . ? C2 C1 O1 121.7(7) . . ? C2 C1 C9 123.5(7) . . ? O1 C1 C9 114.7(7) . . ? C1 C2 C3 117.5(7) . . ? C1 C2 Ni 120.2(6) . . ? C3 C2 Ni 122.3(6) . . ? C4 C3 O2 120.6(7) . . ? C4 C3 C2 123.4(7) . . ? O2 C3 C2 116.0(7) . . ? C3 C4 C10 118.9(7) . . ? C6 C5 C10 121.2(9) . . ? C6 C5 Fe 70.8(6) . . ? C10 C5 Fe 73.8(5) . . ? C5 C6 C7 119.3(9) . . ? C5 C6 Fe 70.3(5) . . ? C7 C6 Fe 69.5(6) . . ? C6 C7 C8 122.0(9) . . ? C6 C7 Fe 70.9(6) . . ? C8 C7 Fe 71.1(5) . . ? C7 C8 C9 118.0(9) . . ? C7 C8 Fe 69.3(5) . . ? C9 C8 Fe 71.9(5) . . ? C8 C9 C10 121.9(7) . . ? C8 C9 C1 122.9(8) . . ? C10 C9 C1 115.1(7) . . ? C8 C9 Fe 69.0(5) . . ? C10 C9 Fe 72.5(4) . . ? C1 C9 Fe 129.1(5) . . ? C9 C10 C4 121.4(7) . . ? C9 C10 C5 117.3(8) . . ? C4 C10 C5 121.0(8) . . ? C9 C10 Fe 69.0(4) . . ? C4 C10 Fe 131.8(6) . . ? C5 C10 Fe 66.5(5) . . ? C12 C11 C15 111.6(15) . . ? C12 C11 Fe 71.5(8) . . ? C15 C11 Fe 70.5(7) . . ? C11 C12 C13 108.0(13) . . ? C11 C12 Fe 70.2(8) . . ? C13 C12 Fe 70.3(6) . . ? C12 C13 C14 106.2(12) . . ? C12 C13 Fe 70.0(7) . . ? C14 C13 Fe 69.4(6) . . ? C15 C14 C13 107.6(11) . . ? C15 C14 Fe 69.5(6) . . ? C13 C14 Fe 70.2(5) . . ? C11 C15 C14 106.6(12) . . ? C11 C15 Fe 70.6(6) . . ? C14 C15 Fe 70.4(6) . . ? C18A C16 C18 106.0(14) . . ? C18A C16 C17 93.8(16) . . ? C18 C16 C17 114.7(13) . . ? C18A C16 C17A 115.5(11) . . ? C18 C16 C17A 101.6(18) . . ? C18A C16 P1 111.0(9) . . ? C18 C16 P1 116.5(11) . . ? C17 C16 P1 112.1(16) . . ? C17A C16 P1 106.1(12) . . ? C20 C19 C20A 93.7(15) . . ? C20 C19 C21A 108(3) . . ? C20A C19 C21A 115.4(15) . . ? C20 C19 C21 115.4(14) . . ? C20A C19 C21 115(2) . . ? C20 C19 P1 114.2(9) . . ? C20A C19 P1 110.3(13) . . ? C21A C19 P1 114(3) . . ? C21 C19 P1 107.5(15) . . ? C23A C22 C24A 116.7(14) . . ? C24A C22 C24 86.0(15) . . ? C23A C22 C23 73.3(18) . . ? C24A C22 C23 113.2(14) . . ? C24 C22 C23 111.9(9) . . ? C23A C22 P2 113.7(17) . . ? C24A C22 P2 116.1(13) . . ? C24 C22 P2 108.3(8) . . ? C23 C22 P2 117.0(8) . . ? C27 C25 C27A 77(2) . . ? C27 C25 C26A 95(3) . . ? C27A C25 C26A 114.6(15) . . ? C27 C25 C26 115.4(10) . . ? C27A C25 C26 98(2) . . ? C27 C25 P2 111.6(9) . . ? C27A C25 P2 140(2) . . ? C26A C25 P2 104(2) . . ? C26 C25 P2 111.5(9) . . ? F1 P3 F3A 119.4(8) . . ? F1 P3 F5 91.2(6) . . ? F3A P3 F5 128.5(8) . . ? F1 P3 F3 91.8(6) . . ? F3A P3 F3 123.4(8) . . ? F5 P3 F3 92.9(6) . . ? F1 P3 F5A 77.3(9) . . ? F3A P3 F5A 90.7(7) . . ? F5 P3 F5A 138.6(7) . . ? F3A P3 F4A 88.7(7) . . ? F5 P3 F4A 100.6(9) . . ? F3 P3 F4A 123.7(8) . . ? F5A P3 F4A 91.9(7) . . ? F1 P3 F2A 102.3(9) . . ? F3A P3 F2A 92.5(7) . . ? F3 P3 F2A 127.9(8) . . ? F5A P3 F2A 176.6(8) . . ? F4A P3 F2A 89.5(7) . . ? F1 P3 F1A 147.7(8) . . ? F3A P3 F1A 90.2(7) . . ? F5 P3 F1A 78.3(9) . . ? F3 P3 F1A 58.8(8) . . ? F5A P3 F1A 90.5(7) . . ? F4A P3 F1A 177.4(8) . . ? F2A P3 F1A 88.1(7) . . ? F1 P3 F6A 60.1(8) . . ? F3A P3 F6A 179.1(8) . . ? F5 P3 F6A 52.4(7) . . ? F3 P3 F6A 56.2(7) . . ? F5A P3 F6A 88.5(7) . . ? F4A P3 F6A 90.9(7) . . ? F2A P3 F6A 88.4(7) . . ? F1A P3 F6A 90.2(7) . . ? F1 P3 F4 178.8(6) . . ? F3A P3 F4 60.6(7) . . ? F5 P3 F4 88.0(6) . . ? F3 P3 F4 89.1(6) . . ? F5A P3 F4 103.9(9) . . ? F4A P3 F4 145.1(7) . . ? F2A P3 F4 76.5(9) . . ? F6A P3 F4 120.0(7) . . ? F1 P3 F2 90.8(6) . . ? F3A P3 F2 47.1(7) . . ? F5 P3 F2 175.5(6) . . ? F3 P3 F2 91.1(6) . . ? F5A P3 F2 45.9(6) . . ? F4A P3 F2 78.9(9) . . ? F2A P3 F2 137.6(7) . . ? F1A P3 F2 102.0(9) . . ? F6A P3 F2 132.0(7) . . ? F4 P3 F2 89.9(6) . . ? F1 P3 F6 92.6(6) . . ? F3A P3 F6 51.4(7) . . ? F5 P3 F6 90.3(6) . . ? F3 P3 F6 174.6(6) . . ? F5A P3 F6 129.3(8) . . ? F4A P3 F6 59.9(7) . . ? F2A P3 F6 54.0(7) . . ? F1A P3 F6 117.7(8) . . ? F6A P3 F6 129.0(7) . . ? F4 P3 F6 86.5(6) . . ? F2 P3 F6 85.6(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.861 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.095 #============================================================================== data_compound-5b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl F6 Fe O2 P3 Pd' _chemical_formula_sum 'C27 H38 Cl F6 Fe O2 P3 Pd' _chemical_formula_weight 799.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.074(2) _cell_length_b 13.2009(16) _cell_length_c 29.002(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6536.7(14) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4971 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 20.85 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.6436 _exptl_absorpt_correction_T_max 0.9493 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 51213 _diffrn_reflns_av_R_equivalents 0.1807 _diffrn_reflns_av_sigmaI/netI 0.1473 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.38 _reflns_number_total 5991 _reflns_number_gt 2362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _publ_section_exptl_refinement ;The isopropyl fragments and PF~6~ are disordered and were modelled in two major contributors, using a free variable for site occupational factor (SOF). The ratio of SOF for isopropyl gruops was 0.50/0.50, 0.52/0.48, 0.83/0.17, 0.62/0.37 and for PF~6~ anion was 0.58/0.42, respectively. The R int and R sigma are high because the crystal sample looses crystallinity during the collecting process. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5991 _refine_ls_number_parameters 501 _refine_ls_number_restraints 583 _refine_ls_R_factor_all 0.1955 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1899 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.48404(5) 0.85113(7) 0.81671(3) 0.0585(3) Uani 1 1 d . . . Fe Fe 0.17422(9) 0.80515(13) 0.90352(6) 0.0665(5) Uani 1 1 d . . . Cl Cl 0.59121(18) 0.8347(3) 0.76547(11) 0.0998(12) Uani 1 1 d . . . P1 P 0.38599(17) 0.8494(3) 0.76363(10) 0.0658(9) Uani 1 1 d . A . O1 O 0.3059(4) 0.8696(6) 0.7947(3) 0.075(2) Uani 1 1 d . . . O2 O 0.4795(4) 0.8788(7) 0.9238(2) 0.089(3) Uani 1 1 d . . . C1 C 0.3216(7) 0.8821(8) 0.8413(4) 0.064(3) Uani 1 1 d . . . C2 C 0.3944(7) 0.8725(8) 0.8577(3) 0.062(3) Uani 1 1 d . . . C3 C 0.4054(6) 0.8824(8) 0.9077(4) 0.063(3) Uani 1 1 d . . . C4 C 0.3446(7) 0.8985(9) 0.9361(4) 0.076(4) Uani 1 1 d . . . H4 H 0.3534 0.9019 0.9677 0.091 Uiso 1 1 calc R . . C5 C 0.2000(7) 0.9217(9) 0.9467(4) 0.082(4) Uani 1 1 d . . . H5 H 0.2062 0.9182 0.9785 0.098 Uiso 1 1 calc R . . C6 C 0.1265(8) 0.9372(10) 0.9297(5) 0.092(4) Uani 1 1 d . . . H6 H 0.0849 0.9518 0.9494 0.110 Uiso 1 1 calc R . . C7 C 0.1152(8) 0.9308(10) 0.8835(5) 0.094(4) Uani 1 1 d . . . H7 H 0.0648 0.9384 0.8718 0.113 Uiso 1 1 calc R . . C8 C 0.1761(7) 0.9136(8) 0.8532(4) 0.077(4) Uani 1 1 d . . . H8 H 0.1666 0.9086 0.8217 0.093 Uiso 1 1 calc R . . C9 C 0.2529(7) 0.9037(8) 0.8705(4) 0.064(3) Uani 1 1 d . . . C10 C 0.2669(6) 0.9106(9) 0.9190(4) 0.064(3) Uani 1 1 d . . . C11 C 0.2261(11) 0.6698(11) 0.8982(9) 0.124(7) Uani 1 1 d . . . H11 H 0.2792 0.6601 0.8927 0.148 Uiso 1 1 calc R . . C12 C 0.1909(11) 0.6783(10) 0.9408(6) 0.101(5) Uani 1 1 d . . . H12 H 0.2165 0.6742 0.9690 0.122 Uiso 1 1 calc R . . C13 C 0.1103(9) 0.6940(11) 0.9348(7) 0.104(5) Uani 1 1 d . . . H13 H 0.0728 0.7039 0.9576 0.124 Uiso 1 1 calc R . . C14 C 0.0987(11) 0.6916(13) 0.8874(8) 0.127(7) Uani 1 1 d . . . H14 H 0.0507 0.6981 0.8726 0.153 Uiso 1 1 calc R . . C15 C 0.1697(18) 0.6781(14) 0.8661(7) 0.147(8) Uani 1 1 d . . . H15 H 0.1775 0.6752 0.8344 0.177 Uiso 1 1 calc R . . C16 C 0.3777(7) 0.9480(10) 0.7219(4) 0.096(4) Uani 1 1 d DU . . H16 H 0.4172 0.9293 0.6989 0.115 Uiso 0.490(14) 1 calc PR A 1 H16A H 0.3288 0.9387 0.7048 0.115 Uiso 0.510(14) 1 calc PR A 2 C17 C 0.3038(11) 0.955(2) 0.6940(8) 0.108(7) Uani 0.490(14) 1 d PDU A 1 H17A H 0.2889 0.8886 0.6838 0.162 Uiso 0.490(14) 1 calc PR A 1 H17B H 0.3125 0.9978 0.6677 0.162 Uiso 0.490(14) 1 calc PR A 1 H17C H 0.2627 0.9830 0.7127 0.162 Uiso 0.490(14) 1 calc PR A 1 C18 C 0.4049(17) 1.0504(15) 0.7380(11) 0.103(7) Uani 0.490(14) 1 d PDU A 1 H18A H 0.4533 1.0433 0.7546 0.155 Uiso 0.490(14) 1 calc PR A 1 H18B H 0.3660 1.0796 0.7579 0.155 Uiso 0.490(14) 1 calc PR A 1 H18C H 0.4129 1.0938 0.7119 0.155 Uiso 0.490(14) 1 calc PR A 1 C17A C 0.4442(13) 0.952(2) 0.6882(7) 0.116(8) Uani 0.510(14) 1 d PDU A 2 H17D H 0.4466 0.8895 0.6714 0.175 Uiso 0.510(14) 1 calc PR A 2 H17E H 0.4925 0.9621 0.7046 0.175 Uiso 0.510(14) 1 calc PR A 2 H17F H 0.4361 1.0071 0.6672 0.175 Uiso 0.510(14) 1 calc PR A 2 C18A C 0.3720(19) 1.0446(16) 0.7496(10) 0.103(7) Uani 0.510(14) 1 d PDU A 2 H18D H 0.3283 1.0405 0.7703 0.155 Uiso 0.510(14) 1 calc PR A 2 H18E H 0.3650 1.1010 0.7291 0.155 Uiso 0.510(14) 1 calc PR A 2 H18F H 0.4193 1.0539 0.7670 0.155 Uiso 0.510(14) 1 calc PR A 2 C19 C 0.3662(7) 0.7287(10) 0.7363(4) 0.098(4) Uani 1 1 d DU . . H19 H 0.3168 0.7384 0.7197 0.117 Uiso 0.518(15) 1 calc PR A 1 H19A H 0.4095 0.7223 0.7144 0.117 Uiso 0.482(15) 1 calc PR A 2 C20 C 0.349(2) 0.652(2) 0.7718(11) 0.109(7) Uani 0.518(15) 1 d PDU A 1 H20A H 0.3079 0.6767 0.7916 0.164 Uiso 0.518(15) 1 calc PR A 1 H20B H 0.3952 0.6398 0.7898 0.164 Uiso 0.518(15) 1 calc PR A 1 H20C H 0.3325 0.5905 0.7573 0.164 Uiso 0.518(15) 1 calc PR A 1 C21 C 0.4244(13) 0.707(2) 0.7005(7) 0.118(8) Uani 0.518(15) 1 d PDU A 1 H21A H 0.4279 0.7643 0.6800 0.177 Uiso 0.518(15) 1 calc PR A 1 H21B H 0.4089 0.6483 0.6835 0.177 Uiso 0.518(15) 1 calc PR A 1 H21C H 0.4745 0.6959 0.7146 0.177 Uiso 0.518(15) 1 calc PR A 1 C20A C 0.380(2) 0.643(2) 0.7678(13) 0.110(8) Uani 0.482(15) 1 d PDU A 2 H20D H 0.4290 0.6522 0.7833 0.164 Uiso 0.482(15) 1 calc PR A 2 H20E H 0.3808 0.5812 0.7505 0.164 Uiso 0.482(15) 1 calc PR A 2 H20F H 0.3384 0.6404 0.7902 0.164 Uiso 0.482(15) 1 calc PR A 2 C21A C 0.2975(12) 0.729(2) 0.7062(8) 0.108(8) Uani 0.482(15) 1 d PDU A 2 H21D H 0.3001 0.7869 0.6859 0.162 Uiso 0.482(15) 1 calc PR A 2 H21E H 0.2509 0.7337 0.7246 0.162 Uiso 0.482(15) 1 calc PR A 2 H21F H 0.2964 0.6683 0.6883 0.162 Uiso 0.482(15) 1 calc PR A 2 C22 C 0.5837(7) 0.7356(10) 0.9089(6) 0.115(4) Uani 1 1 d DU . . H22 H 0.5963 0.7458 0.9415 0.138 Uiso 0.825(15) 1 calc PR B 1 H22A H 0.6122 0.7056 0.8829 0.138 Uiso 0.175(15) 1 calc PR B 2 C23 C 0.5248(11) 0.6513(15) 0.9053(11) 0.142(7) Uani 0.825(15) 1 d PDU B 1 H23A H 0.4779 0.6700 0.9215 0.214 Uiso 0.825(15) 1 calc PR B 1 H23B H 0.5462 0.5908 0.9187 0.214 Uiso 0.825(15) 1 calc PR B 1 H23C H 0.5127 0.6393 0.8735 0.214 Uiso 0.825(15) 1 calc PR B 1 C24 C 0.6564(9) 0.7044(13) 0.8843(6) 0.119(6) Uani 0.825(15) 1 d PDU B 1 H24A H 0.6950 0.7569 0.8871 0.178 Uiso 0.825(15) 1 calc PR B 1 H24B H 0.6449 0.6931 0.8524 0.178 Uiso 0.825(15) 1 calc PR B 1 H24C H 0.6763 0.6431 0.8978 0.178 Uiso 0.825(15) 1 calc PR B 1 C23A C 0.508(4) 0.679(7) 0.909(5) 0.127(9) Uani 0.175(15) 1 d PDU B 2 H23D H 0.4789 0.6940 0.8817 0.191 Uiso 0.175(15) 1 calc PR B 2 H23E H 0.4776 0.6988 0.9357 0.191 Uiso 0.175(15) 1 calc PR B 2 H23F H 0.5180 0.6075 0.9107 0.191 Uiso 0.175(15) 1 calc PR B 2 C24A C 0.631(4) 0.705(5) 0.9498(17) 0.111(11) Uani 0.175(15) 1 d PDU B 2 H24D H 0.6789 0.7426 0.9505 0.166 Uiso 0.175(15) 1 calc PR B 2 H24E H 0.6425 0.6337 0.9480 0.166 Uiso 0.175(15) 1 calc PR B 2 H24F H 0.6016 0.7180 0.9775 0.166 Uiso 0.175(15) 1 calc PR B 2 P2 P 0.54794(17) 0.8515(3) 0.88617(10) 0.0683(9) Uani 1 1 d . B . C25 C 0.6182(9) 0.9510(14) 0.8992(5) 0.127(5) Uani 1 1 d DU . . H25 H 0.6691 0.9302 0.8868 0.152 Uiso 0.623(17) 1 calc PR B 1 H25A H 0.5851 1.0110 0.8951 0.152 Uiso 0.377(17) 1 calc PR B 2 C26 C 0.628(2) 0.974(4) 0.9478(5) 0.136(8) Uani 0.623(17) 1 d PDU B 1 H26A H 0.6448 0.9143 0.9640 0.205 Uiso 0.623(17) 1 calc PR B 1 H26B H 0.5798 0.9978 0.9605 0.205 Uiso 0.623(17) 1 calc PR B 1 H26C H 0.6677 1.0258 0.9512 0.205 Uiso 0.623(17) 1 calc PR B 1 C27 C 0.5965(15) 1.0453(17) 0.8772(8) 0.147(8) Uani 0.623(17) 1 d PDU B 1 H27A H 0.5881 1.0339 0.8449 0.220 Uiso 0.623(17) 1 calc PR B 1 H27B H 0.6378 1.0939 0.8812 0.220 Uiso 0.623(17) 1 calc PR B 1 H27C H 0.5492 1.0707 0.8909 0.220 Uiso 0.623(17) 1 calc PR B 1 C26A C 0.6779(17) 0.971(3) 0.8649(9) 0.125(9) Uani 0.377(17) 1 d PDU B 2 H26D H 0.6600 0.9475 0.8353 0.187 Uiso 0.377(17) 1 calc PR B 2 H26E H 0.7250 0.9351 0.8731 0.187 Uiso 0.377(17) 1 calc PR B 2 H26F H 0.6883 1.0419 0.8636 0.187 Uiso 0.377(17) 1 calc PR B 2 C27A C 0.653(4) 0.974(6) 0.9436(7) 0.135(8) Uani 0.377(17) 1 d PDU B 2 H27D H 0.6150 0.9654 0.9675 0.203 Uiso 0.377(17) 1 calc PR B 2 H27E H 0.6722 1.0421 0.9436 0.203 Uiso 0.377(17) 1 calc PR B 2 H27F H 0.6964 0.9282 0.9490 0.203 Uiso 0.377(17) 1 calc PR B 2 P3 P -0.1186(2) 0.8382(3) 0.95322(15) 0.1077(13) Uani 1 1 d DU . . F1 F -0.1760(7) 0.9104(9) 0.9306(5) 0.184(4) Uani 0.582(8) 1 d PDU C 1 F2 F -0.1449(7) 0.8705(11) 1.0022(3) 0.153(4) Uani 0.582(8) 1 d PDU C 1 F3 F -0.0567(6) 0.9211(7) 0.9528(6) 0.165(4) Uani 0.582(8) 1 d PDU C 1 F4 F -0.0616(7) 0.7642(9) 0.9772(4) 0.152(4) Uani 0.582(8) 1 d PDU C 1 F5 F -0.0920(8) 0.8032(12) 0.9060(3) 0.167(4) Uani 0.582(8) 1 d PDU C 1 F6 F -0.1811(6) 0.7542(8) 0.9558(6) 0.157(4) Uani 0.582(8) 1 d PDU C 1 F1A F -0.0736(9) 0.7383(8) 0.9516(7) 0.159(5) Uani 0.418(8) 1 d PDU C 2 F2A F -0.0611(8) 0.8823(14) 0.9887(5) 0.152(4) Uani 0.418(8) 1 d PDU C 2 F3A F -0.0657(9) 0.8772(15) 0.9136(5) 0.148(5) Uani 0.418(8) 1 d PDU C 2 F4A F -0.1624(9) 0.9395(8) 0.9547(7) 0.167(5) Uani 0.418(8) 1 d PDU C 2 F5A F -0.1738(9) 0.7968(14) 0.9164(5) 0.157(4) Uani 0.418(8) 1 d PDU C 2 F6A F -0.1698(9) 0.8009(15) 0.9923(5) 0.175(5) Uani 0.418(8) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0484(5) 0.0766(6) 0.0504(5) -0.0019(5) 0.0073(4) -0.0042(5) Fe 0.0480(9) 0.0750(12) 0.0765(12) -0.0040(10) 0.0051(9) -0.0040(9) Cl 0.072(2) 0.144(3) 0.084(2) -0.002(2) 0.0253(18) 0.007(2) P1 0.0614(19) 0.088(2) 0.0485(18) 0.0010(19) 0.0044(14) -0.0053(19) O1 0.055(5) 0.112(7) 0.057(5) -0.007(5) 0.000(4) 0.004(4) O2 0.049(4) 0.158(8) 0.060(5) -0.006(5) -0.012(4) -0.005(5) C1 0.058(8) 0.067(8) 0.066(8) -0.002(7) 0.004(7) -0.007(6) C2 0.066(8) 0.077(9) 0.044(7) 0.005(6) 0.001(6) -0.008(7) C3 0.055(7) 0.082(9) 0.053(8) -0.006(6) 0.011(6) 0.004(6) C4 0.066(8) 0.109(10) 0.052(7) -0.014(7) -0.002(7) -0.021(7) C5 0.048(8) 0.110(11) 0.087(10) -0.016(8) 0.016(7) -0.001(7) C6 0.069(10) 0.106(12) 0.100(12) -0.009(10) 0.034(9) 0.008(8) C7 0.081(10) 0.103(11) 0.097(12) -0.015(9) 0.042(9) -0.011(8) C8 0.068(9) 0.072(9) 0.092(10) 0.004(7) -0.006(8) 0.016(7) C9 0.056(7) 0.053(7) 0.082(9) -0.002(7) -0.004(8) 0.000(6) C10 0.061(8) 0.072(9) 0.059(8) -0.001(6) 0.001(6) -0.009(7) C11 0.103(14) 0.059(11) 0.21(2) 0.005(13) 0.046(15) 0.033(9) C12 0.113(14) 0.097(12) 0.094(12) 0.010(9) -0.019(10) 0.004(10) C13 0.057(10) 0.105(11) 0.149(16) 0.018(11) 0.025(10) -0.015(8) C14 0.113(15) 0.127(14) 0.142(18) 0.006(14) -0.041(13) -0.053(12) C15 0.21(3) 0.109(16) 0.124(17) -0.045(13) 0.014(19) -0.052(18) C16 0.081(8) 0.122(8) 0.086(9) 0.019(8) -0.003(6) -0.001(8) C17 0.095(14) 0.155(17) 0.074(15) 0.033(13) -0.009(10) 0.001(13) C18 0.097(17) 0.108(10) 0.104(15) 0.046(11) 0.002(12) -0.017(12) C17A 0.097(15) 0.152(17) 0.100(16) 0.028(13) 0.012(10) 0.007(14) C18A 0.097(16) 0.099(11) 0.113(15) 0.029(10) 0.014(12) -0.007(13) C19 0.089(9) 0.108(9) 0.097(10) -0.020(7) -0.011(6) 0.002(8) C20 0.102(18) 0.089(13) 0.137(14) -0.017(10) 0.005(12) -0.008(14) C21 0.128(17) 0.138(17) 0.088(15) -0.036(12) -0.005(10) 0.013(14) C20A 0.103(18) 0.085(13) 0.141(15) -0.015(10) -0.006(13) 0.001(14) C21A 0.094(15) 0.126(17) 0.105(16) -0.039(13) -0.018(10) -0.013(14) C22 0.114(10) 0.091(10) 0.141(11) 0.027(9) -0.016(8) 0.011(7) C23 0.156(13) 0.090(13) 0.181(14) 0.033(13) -0.008(12) -0.009(10) C24 0.111(10) 0.097(12) 0.149(14) 0.012(11) -0.034(10) 0.038(9) C23A 0.126(15) 0.093(18) 0.163(17) 0.028(17) -0.012(15) 0.000(13) C24A 0.11(2) 0.08(2) 0.14(2) 0.03(2) -0.005(16) 0.030(19) P2 0.0502(17) 0.096(2) 0.0583(19) -0.0055(19) 0.0000(15) -0.0070(19) C25 0.105(10) 0.177(13) 0.097(9) -0.019(10) -0.021(8) -0.043(10) C26 0.111(17) 0.199(15) 0.099(10) -0.032(11) -0.003(12) -0.054(15) C27 0.139(17) 0.164(17) 0.137(14) -0.015(13) -0.035(15) -0.055(16) C26A 0.105(18) 0.17(2) 0.095(13) -0.006(19) -0.027(12) -0.050(18) C27A 0.111(19) 0.196(17) 0.099(11) -0.031(14) -0.018(11) -0.043(17) P3 0.066(2) 0.120(3) 0.137(3) -0.013(3) 0.021(2) 0.0016(19) F1 0.144(7) 0.166(9) 0.243(10) -0.009(8) -0.045(8) 0.035(6) F2 0.136(8) 0.154(9) 0.170(6) -0.063(6) 0.043(6) -0.025(7) F3 0.125(7) 0.177(8) 0.192(11) 0.001(8) 0.010(8) -0.054(6) F4 0.137(7) 0.166(8) 0.153(9) -0.017(8) -0.016(7) 0.037(6) F5 0.179(9) 0.192(10) 0.131(6) -0.019(6) 0.020(6) 0.015(8) F6 0.139(7) 0.163(8) 0.170(10) -0.037(7) -0.005(7) -0.056(6) F1A 0.160(10) 0.145(7) 0.172(12) -0.020(7) 0.014(8) 0.043(7) F2A 0.127(8) 0.179(10) 0.150(8) -0.030(8) -0.006(7) -0.013(7) F3A 0.138(9) 0.162(11) 0.145(8) -0.025(8) 0.037(7) -0.051(8) F4A 0.164(10) 0.147(7) 0.188(12) -0.031(7) -0.002(8) 0.047(7) F5A 0.119(8) 0.163(10) 0.189(9) -0.023(8) -0.016(7) -0.032(8) F6A 0.160(9) 0.180(11) 0.185(8) -0.019(9) 0.079(7) -0.034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C2 1.960(11) . ? Pd P1 2.274(3) . ? Pd P2 2.291(3) . ? Pd Cl 2.367(3) . ? Fe C15 2.000(17) . ? Fe C11 2.001(13) . ? Fe C12 2.013(13) . ? Fe C7 2.026(14) . ? Fe C14 2.032(15) . ? Fe C5 2.032(12) . ? Fe C13 2.041(13) . ? Fe C8 2.045(12) . ? Fe C6 2.069(13) . ? Fe C9 2.100(11) . ? Fe C10 2.155(11) . ? P1 O1 1.658(7) . ? P1 C16 1.783(13) . ? P1 C19 1.811(13) . ? O1 C1 1.390(12) . ? O2 C3 1.349(11) . ? O2 P2 1.640(8) . ? C1 C2 1.336(14) . ? C1 C9 1.475(14) . ? C2 C3 1.465(14) . ? C3 C4 1.344(13) . ? C4 C10 1.427(14) . ? C5 C6 1.365(15) . ? C5 C10 1.404(14) . ? C6 C7 1.357(16) . ? C7 C8 1.380(14) . ? C8 C9 1.410(14) . ? C9 C10 1.428(14) . ? C11 C15 1.34(2) . ? C11 C12 1.38(2) . ? C12 C13 1.401(18) . ? C13 C14 1.39(2) . ? C14 C15 1.37(2) . ? C16 C17A 1.498(13) . ? C16 C17 1.502(13) . ? C16 C18 1.505(13) . ? C16 C18A 1.511(13) . ? C19 C21A 1.462(13) . ? C19 C21 1.464(13) . ? C19 C20A 1.470(13) . ? C19 C20 1.471(13) . ? C22 C24 1.490(13) . ? C22 C24A 1.491(15) . ? C22 C23A 1.497(15) . ? C22 C23 1.503(13) . ? C22 P2 1.774(14) . ? P2 C25 1.818(15) . ? C25 C27 1.447(14) . ? C25 C26A 1.447(14) . ? C25 C27A 1.453(14) . ? C25 C26 1.455(14) . ? P3 F6A 1.513(7) . ? P3 F1 1.516(6) . ? P3 F5 1.516(6) . ? P3 F3 1.521(6) . ? P3 F5A 1.525(7) . ? P3 F1A 1.527(7) . ? P3 F4A 1.533(7) . ? P3 F2A 1.536(7) . ? P3 F6 1.540(6) . ? P3 F4 1.544(6) . ? P3 F2 1.548(6) . ? P3 F3A 1.549(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd P1 80.6(3) . . ? C2 Pd P2 80.7(3) . . ? P1 Pd P2 161.04(11) . . ? C2 Pd Cl 176.7(3) . . ? P1 Pd Cl 98.23(11) . . ? P2 Pd Cl 100.61(12) . . ? C15 Fe C11 39.3(7) . . ? C15 Fe C12 66.4(7) . . ? C11 Fe C12 40.2(6) . . ? C15 Fe C7 120.8(9) . . ? C11 Fe C7 158.4(9) . . ? C12 Fe C7 154.9(7) . . ? C15 Fe C14 39.8(7) . . ? C11 Fe C14 66.7(8) . . ? C12 Fe C14 66.4(6) . . ? C7 Fe C14 102.9(7) . . ? C15 Fe C5 168.0(10) . . ? C11 Fe C5 128.9(9) . . ? C12 Fe C5 105.6(6) . . ? C7 Fe C5 70.4(5) . . ? C14 Fe C5 146.9(8) . . ? C15 Fe C13 67.6(8) . . ? C11 Fe C13 68.2(6) . . ? C12 Fe C13 40.4(5) . . ? C7 Fe C13 116.8(6) . . ? C14 Fe C13 39.9(6) . . ? C5 Fe C13 112.7(6) . . ? C15 Fe C8 101.5(7) . . ? C11 Fe C8 124.3(8) . . ? C12 Fe C8 164.4(7) . . ? C7 Fe C8 39.6(4) . . ? C14 Fe C8 111.3(7) . . ? C5 Fe C8 84.6(5) . . ? C13 Fe C8 146.0(6) . . ? C15 Fe C6 153.0(10) . . ? C11 Fe C6 162.8(9) . . ? C12 Fe C6 124.0(7) . . ? C7 Fe C6 38.7(4) . . ? C14 Fe C6 117.1(8) . . ? C5 Fe C6 38.9(4) . . ? C13 Fe C6 103.4(6) . . ? C8 Fe C6 71.3(5) . . ? C15 Fe C9 107.3(7) . . ? C11 Fe C9 103.6(6) . . ? C12 Fe C9 132.0(6) . . ? C7 Fe C9 71.3(5) . . ? C14 Fe C9 139.3(8) . . ? C5 Fe C9 70.9(5) . . ? C13 Fe C9 171.7(5) . . ? C8 Fe C9 39.7(4) . . ? C6 Fe C9 84.1(5) . . ? C15 Fe C10 133.1(9) . . ? C11 Fe C10 105.6(7) . . ? C12 Fe C10 108.8(5) . . ? C7 Fe C10 84.0(5) . . ? C14 Fe C10 172.2(7) . . ? C5 Fe C10 39.0(4) . . ? C13 Fe C10 139.8(7) . . ? C8 Fe C10 71.6(5) . . ? C6 Fe C10 70.6(5) . . ? C9 Fe C10 39.2(4) . . ? O1 P1 C16 100.7(5) . . ? O1 P1 C19 103.0(5) . . ? C16 P1 C19 109.3(6) . . ? O1 P1 Pd 103.7(3) . . ? C16 P1 Pd 120.7(4) . . ? C19 P1 Pd 116.3(4) . . ? C1 O1 P1 112.9(7) . . ? C3 O2 P2 116.4(7) . . ? C2 C1 O1 121.0(10) . . ? C2 C1 C9 123.6(11) . . ? O1 C1 C9 115.4(10) . . ? C1 C2 C3 117.6(10) . . ? C1 C2 Pd 121.6(8) . . ? C3 C2 Pd 120.8(8) . . ? C4 C3 O2 121.1(10) . . ? C4 C3 C2 121.4(10) . . ? O2 C3 C2 117.4(9) . . ? C3 C4 C10 121.5(11) . . ? C6 C5 C10 123.9(12) . . ? C6 C5 Fe 72.0(8) . . ? C10 C5 Fe 75.2(7) . . ? C7 C6 C5 118.5(13) . . ? C7 C6 Fe 68.9(8) . . ? C5 C6 Fe 69.1(7) . . ? C6 C7 C8 122.2(14) . . ? C6 C7 Fe 72.4(9) . . ? C8 C7 Fe 70.9(8) . . ? C7 C8 C9 119.2(12) . . ? C7 C8 Fe 69.4(8) . . ? C9 C8 Fe 72.3(7) . . ? C8 C9 C10 120.0(11) . . ? C8 C9 C1 123.5(11) . . ? C10 C9 C1 116.4(10) . . ? C8 C9 Fe 68.0(7) . . ? C10 C9 Fe 72.5(7) . . ? C1 C9 Fe 130.6(8) . . ? C5 C10 C4 124.7(11) . . ? C5 C10 C9 115.7(11) . . ? C4 C10 C9 119.4(10) . . ? C5 C10 Fe 65.7(7) . . ? C4 C10 Fe 133.1(9) . . ? C9 C10 Fe 68.3(6) . . ? C15 C11 C12 107.5(18) . . ? C15 C11 Fe 70.3(10) . . ? C12 C11 Fe 70.4(8) . . ? C11 C12 C13 109.3(15) . . ? C11 C12 Fe 69.4(8) . . ? C13 C12 Fe 70.9(8) . . ? C14 C13 C12 105.0(14) . . ? C14 C13 Fe 69.7(9) . . ? C12 C13 Fe 68.7(8) . . ? C15 C14 C13 108.9(18) . . ? C15 C14 Fe 68.8(10) . . ? C13 C14 Fe 70.4(9) . . ? C11 C15 C14 109(2) . . ? C11 C15 Fe 70.4(10) . . ? C14 C15 Fe 71.3(11) . . ? C17A C16 C17 106.5(16) . . ? C17A C16 C18 86.4(16) . . ? C17 C16 C18 111.8(16) . . ? C17A C16 C18A 111.4(15) . . ? C17 C16 C18A 100(2) . . ? C18 C16 C18A 25.2(17) . . ? C17A C16 P1 114.1(13) . . ? C17 C16 P1 118.5(13) . . ? C18 C16 P1 114.9(15) . . ? C18A C16 P1 105.1(15) . . ? C21A C19 C21 97.0(17) . . ? C21A C19 C20A 120.2(18) . . ? C21 C19 C20A 101(2) . . ? C21A C19 C20 105(2) . . ? C21 C19 C20 120.1(17) . . ? C20A C19 C20 22(2) . . ? C21A C19 P1 113.9(14) . . ? C21 C19 P1 110.6(14) . . ? C20A C19 P1 112.0(18) . . ? C20 C19 P1 109.5(17) . . ? C24 C22 C24A 82(3) . . ? C24 C22 C23A 126(6) . . ? C24A C22 C23A 109(2) . . ? C24 C22 C23 108.7(17) . . ? C24A C22 C23 102(3) . . ? C23A C22 C23 18(6) . . ? C24 C22 P2 110.3(10) . . ? C24A C22 P2 136(3) . . ? C23A C22 P2 98(3) . . ? C23 C22 P2 112.5(12) . . ? O2 P2 C22 100.8(6) . . ? O2 P2 C25 100.0(6) . . ? C22 P2 C25 108.6(7) . . ? O2 P2 Pd 104.3(3) . . ? C22 P2 Pd 119.3(6) . . ? C25 P2 Pd 119.9(5) . . ? C27 C25 C26A 74.0(19) . . ? C27 C25 C27A 109(4) . . ? C26A C25 C27A 106(2) . . ? C27 C25 C26 106(2) . . ? C26A C25 C26 123(2) . . ? C27A C25 C26 18(4) . . ? C27 C25 P2 111.2(14) . . ? C26A C25 P2 116.8(17) . . ? C27A C25 P2 127(2) . . ? C26 C25 P2 115.7(17) . . ? F6A P3 F1 98.9(9) . . ? F6A P3 F5 138.7(7) . . ? F1 P3 F5 89.7(5) . . ? F6A P3 F3 129.9(6) . . ? F1 P3 F3 89.7(5) . . ? F5 P3 F3 90.2(5) . . ? F6A P3 F5A 92.9(5) . . ? F1 P3 F5A 61.5(7) . . ? F5 P3 F5A 56.2(6) . . ? F3 P3 F5A 133.0(7) . . ? F6A P3 F1A 92.0(6) . . ? F1 P3 F1A 148.7(7) . . ? F5 P3 F1A 63.7(7) . . ? F3 P3 F1A 105.7(8) . . ? F5A P3 F1A 88.8(5) . . ? F6A P3 F4A 88.9(5) . . ? F1 P3 F4A 31.6(7) . . ? F5 P3 F4A 116.0(7) . . ? F3 P3 F4A 73.2(8) . . ? F5A P3 F4A 91.8(5) . . ? F1A P3 F4A 178.9(5) . . ? F6A P3 F2A 89.5(5) . . ? F1 P3 F2A 117.7(8) . . ? F5 P3 F2A 121.9(7) . . ? F3 P3 F2A 44.6(7) . . ? F5A P3 F2A 177.6(5) . . ? F1A P3 F2A 91.5(5) . . ? F4A P3 F2A 87.8(5) . . ? F6A P3 F6 47.9(6) . . ? F1 P3 F6 91.5(5) . . ? F5 P3 F6 91.9(5) . . ? F3 P3 F6 177.6(5) . . ? F5A P3 F6 49.3(7) . . ? F1A P3 F6 74.3(8) . . ? F4A P3 F6 106.8(8) . . ? F2A P3 F6 133.0(7) . . ? F6A P3 F4 79.7(9) . . ? F1 P3 F4 178.6(5) . . ? F5 P3 F4 91.4(5) . . ? F3 P3 F4 91.2(5) . . ? F5A P3 F4 118.5(7) . . ? F1A P3 F4 31.8(7) . . ? F4A P3 F4 147.9(7) . . ? F2A P3 F4 62.3(7) . . ? F6 P3 F4 87.7(5) . . ? F6A P3 F2 40.2(7) . . ? F1 P3 F2 92.1(5) . . ? F5 P3 F2 178.1(5) . . ? F3 P3 F2 90.6(5) . . ? F5A P3 F2 124.2(6) . . ? F1A P3 F2 114.3(7) . . ? F4A P3 F2 66.0(7) . . ? F2A P3 F2 57.8(6) . . ? F6 P3 F2 87.3(5) . . ? F4 P3 F2 86.8(5) . . ? F6A P3 F3A 179.3(5) . . ? F1 P3 F3A 81.2(9) . . ? F5 P3 F3A 42.0(7) . . ? F3 P3 F3A 49.5(6) . . ? F5A P3 F3A 87.7(5) . . ? F1A P3 F3A 88.3(5) . . ? F4A P3 F3A 90.9(5) . . ? F2A P3 F3A 89.8(5) . . ? F6 P3 F3A 132.8(6) . . ? F4 P3 F3A 100.1(9) . . ? F2 P3 F3A 139.2(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.909 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.106 #============================================================================== data_compound-5c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Cl Fe O2 P2 Pt, F6 P' _chemical_formula_sum 'C27 H38 Cl F6 Fe O2 P3 Pt' _chemical_formula_weight 887.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.0443(12) _cell_length_b 13.1286(9) _cell_length_c 29.024(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6494.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9992 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.93 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 5.039 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.2924 _exptl_absorpt_correction_T_max 0.7155 _exptl_absorpt_process_details 'SHELXTL V 6.12 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 68330 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5944 _reflns_number_gt 3330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5944 _refine_ls_number_parameters 495 _refine_ls_number_restraints 639 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.01727(3) 0.64853(3) 0.182763(14) 0.05900(18) Uani 1 1 d . . . Fe Fe 0.32624(9) 0.69597(13) 0.09553(6) 0.0702(5) Uani 1 1 d . . . P1 P 0.11360(18) 0.6512(2) 0.23607(10) 0.0662(8) Uani 1 1 d . A . P2 P -0.04655(19) 0.6467(3) 0.11379(11) 0.0703(9) Uani 1 1 d . B . Cl Cl -0.0907(2) 0.6640(3) 0.23338(12) 0.0924(11) Uani 1 1 d . . . O1 O 0.1945(4) 0.6307(6) 0.2052(3) 0.078(2) Uani 1 1 d . . . O2 O 0.0207(5) 0.6218(7) 0.0768(3) 0.091(3) Uani 1 1 d . . . C1 C 0.1788(8) 0.6187(8) 0.1582(4) 0.066(3) Uani 1 1 d . . . C2 C 0.1077(7) 0.6267(8) 0.1413(4) 0.063(3) Uani 1 1 d . . . C3 C 0.0952(7) 0.6162(9) 0.0924(4) 0.063(3) Uani 1 1 d . . . C4 C 0.1572(8) 0.6010(10) 0.0636(4) 0.079(4) Uani 1 1 d . . . H4 H 0.1491 0.5986 0.0319 0.095 Uiso 1 1 calc R . . C5 C 0.3014(8) 0.5772(9) 0.0534(5) 0.096(4) Uani 1 1 d . . . H5 H 0.2951 0.5788 0.0215 0.115 Uiso 1 1 calc R . . C6 C 0.3742(8) 0.5641(11) 0.0699(5) 0.097(3) Uani 1 1 d . . . H6 H 0.4158 0.5513 0.0500 0.116 Uiso 1 1 calc R . . C7 C 0.3870(8) 0.5697(10) 0.1178(5) 0.097(3) Uani 1 1 d . . . H7 H 0.4372 0.5619 0.1298 0.116 Uiso 1 1 calc R . . C8 C 0.3246(7) 0.5868(10) 0.1466(5) 0.088(4) Uani 1 1 d . . . H8 H 0.3334 0.5927 0.1781 0.105 Uiso 1 1 calc R . . C9 C 0.2495(7) 0.5954(8) 0.1300(4) 0.066(3) Uani 1 1 d . . . C10 C 0.2328(7) 0.5891(8) 0.0811(4) 0.061(3) Uani 1 1 d . . . C11 C 0.3995(12) 0.8118(13) 0.1116(9) 0.130(7) Uani 1 1 d . . . H11 H 0.4481 0.8043 0.1258 0.156 Uiso 1 1 calc R . . C12 C 0.3327(19) 0.8262(13) 0.1329(8) 0.144(8) Uani 1 1 d . . . H12 H 0.3266 0.8315 0.1647 0.173 Uiso 1 1 calc R . . C13 C 0.2720(12) 0.8323(11) 0.1006(10) 0.128(8) Uani 1 1 d . . . H13 H 0.2189 0.8414 0.1065 0.154 Uiso 1 1 calc R . . C14 C 0.3065(12) 0.8223(11) 0.0590(7) 0.109(5) Uani 1 1 d . . . H14 H 0.2802 0.8236 0.0309 0.131 Uiso 1 1 calc R . . C15 C 0.3865(10) 0.8096(11) 0.0643(7) 0.103(5) Uani 1 1 d . . . H15 H 0.4237 0.8014 0.0412 0.123 Uiso 1 1 calc R . . C16 C 0.1324(8) 0.7727(9) 0.2647(5) 0.100(4) Uani 1 1 d DU . . H16 H 0.0877 0.7817 0.2855 0.120 Uiso 0.513(19) 1 calc PR A 1 H16A H 0.1822 0.7655 0.2813 0.120 Uiso 0.487(19) 1 calc PR A 2 C17 C 0.126(2) 0.861(3) 0.2312(13) 0.109(8) Uani 0.513(19) 1 d PDU A 1 H17A H 0.0779 0.8556 0.2143 0.163 Uiso 0.513(19) 1 calc PR A 1 H17B H 0.1695 0.8587 0.2101 0.163 Uiso 0.513(19) 1 calc PR A 1 H17C H 0.1271 0.9238 0.2479 0.163 Uiso 0.513(19) 1 calc PR A 1 C18 C 0.2014(13) 0.771(2) 0.2953(8) 0.103(8) Uani 0.513(19) 1 d PDU A 1 H18A H 0.1937 0.7203 0.3188 0.155 Uiso 0.513(19) 1 calc PR A 1 H18B H 0.2080 0.8364 0.3093 0.155 Uiso 0.513(19) 1 calc PR A 1 H18C H 0.2473 0.7541 0.2777 0.155 Uiso 0.513(19) 1 calc PR A 1 C17A C 0.0710(16) 0.800(2) 0.3000(9) 0.122(9) Uani 0.487(19) 1 d PDU A 2 H17D H 0.0728 0.7520 0.3249 0.183 Uiso 0.487(19) 1 calc PR A 2 H17E H 0.0200 0.7981 0.2859 0.183 Uiso 0.487(19) 1 calc PR A 2 H17F H 0.0810 0.8672 0.3116 0.183 Uiso 0.487(19) 1 calc PR A 2 C18A C 0.146(3) 0.846(3) 0.2270(13) 0.110(8) Uani 0.487(19) 1 d PDU A 2 H18D H 0.1875 0.8221 0.2075 0.165 Uiso 0.487(19) 1 calc PR A 2 H18E H 0.1605 0.9112 0.2399 0.165 Uiso 0.487(19) 1 calc PR A 2 H18F H 0.0989 0.8540 0.2092 0.165 Uiso 0.487(19) 1 calc PR A 2 C19 C 0.1210(7) 0.5490(9) 0.2774(4) 0.090(4) Uani 1 1 d DU . . H19 H 0.1698 0.5591 0.2947 0.108 Uiso 0.552(18) 1 calc PR A 1 H19A H 0.0811 0.5672 0.3003 0.108 Uiso 0.448(18) 1 calc PR A 2 C20 C 0.1305(16) 0.4523(16) 0.2493(10) 0.100(7) Uani 0.552(18) 1 d PDU A 1 H20A H 0.1727 0.4608 0.2278 0.151 Uiso 0.552(18) 1 calc PR A 1 H20B H 0.0827 0.4387 0.2329 0.151 Uiso 0.552(18) 1 calc PR A 1 H20C H 0.1419 0.3964 0.2695 0.151 Uiso 0.552(18) 1 calc PR A 1 C21 C 0.0560(14) 0.550(2) 0.3110(8) 0.126(8) Uani 0.552(18) 1 d PDU A 1 H21A H 0.0564 0.6138 0.3275 0.189 Uiso 0.552(18) 1 calc PR A 1 H21B H 0.0624 0.4951 0.3324 0.189 Uiso 0.552(18) 1 calc PR A 1 H21C H 0.0070 0.5429 0.2951 0.189 Uiso 0.552(18) 1 calc PR A 1 C20A C 0.0922(18) 0.4471(17) 0.2596(13) 0.100(8) Uani 0.448(18) 1 d PDU A 2 H20D H 0.0438 0.4565 0.2432 0.149 Uiso 0.448(18) 1 calc PR A 2 H20E H 0.0838 0.4017 0.2850 0.149 Uiso 0.448(18) 1 calc PR A 2 H20F H 0.1308 0.4186 0.2392 0.149 Uiso 0.448(18) 1 calc PR A 2 C21A C 0.1942(13) 0.547(2) 0.3049(9) 0.100(8) Uani 0.448(18) 1 d PDU A 2 H21D H 0.2067 0.6153 0.3147 0.150 Uiso 0.448(18) 1 calc PR A 2 H21E H 0.2363 0.5211 0.2864 0.150 Uiso 0.448(18) 1 calc PR A 2 H21F H 0.1871 0.5047 0.3314 0.150 Uiso 0.448(18) 1 calc PR A 2 C22 C -0.0842(9) 0.7640(9) 0.0929(6) 0.112(4) Uani 1 1 d DU . . H22 H -0.0997 0.7497 0.0611 0.135 Uiso 0.802(17) 1 calc PR B 1 H22A H -0.1277 0.7698 0.1148 0.135 Uiso 0.198(17) 1 calc PR B 2 C23 C -0.0209(11) 0.8448(14) 0.0889(9) 0.129(6) Uani 0.802(17) 1 d PDU B 1 H23A H 0.0238 0.8170 0.0731 0.194 Uiso 0.802(17) 1 calc PR B 1 H23B H -0.0055 0.8667 0.1191 0.194 Uiso 0.802(17) 1 calc PR B 1 H23C H -0.0408 0.9019 0.0719 0.194 Uiso 0.802(17) 1 calc PR B 1 C24 C -0.1575(10) 0.7947(13) 0.1161(6) 0.119(6) Uani 0.802(17) 1 d PDU B 1 H24A H -0.1931 0.7380 0.1169 0.178 Uiso 0.802(17) 1 calc PR B 1 H24B H -0.1812 0.8501 0.0996 0.178 Uiso 0.802(17) 1 calc PR B 1 H24C H -0.1460 0.8160 0.1470 0.178 Uiso 0.802(17) 1 calc PR B 1 C23A C -0.031(5) 0.842(4) 0.116(3) 0.122(9) Uani 0.198(17) 1 d PDU B 2 H23D H -0.0061 0.8114 0.1420 0.183 Uiso 0.198(17) 1 calc PR B 2 H23E H -0.0611 0.8995 0.1251 0.183 Uiso 0.198(17) 1 calc PR B 2 H23F H 0.0087 0.8629 0.0941 0.183 Uiso 0.198(17) 1 calc PR B 2 C24A C -0.128(4) 0.798(5) 0.0519(17) 0.116(10) Uani 0.198(17) 1 d PDU B 2 H24D H -0.1675 0.7490 0.0444 0.175 Uiso 0.198(17) 1 calc PR B 2 H24E H -0.0922 0.8050 0.0264 0.175 Uiso 0.198(17) 1 calc PR B 2 H24F H -0.1519 0.8628 0.0581 0.175 Uiso 0.198(17) 1 calc PR B 2 C25 C -0.1167(9) 0.5459(12) 0.1022(5) 0.122(5) Uani 1 1 d DU . . H25 H -0.0834 0.4925 0.1154 0.146 Uiso 0.560(15) 1 calc PR B 2 H25A H -0.1640 0.5638 0.1195 0.146 Uiso 0.440(15) 1 calc PR B 1 C26 C -0.142(2) 0.542(2) 0.0521(7) 0.123(8) Uani 0.560(15) 1 d PDU B 1 H26A H -0.1573 0.6093 0.0424 0.185 Uiso 0.560(15) 1 calc PR B 1 H26B H -0.1849 0.4962 0.0487 0.185 Uiso 0.560(15) 1 calc PR B 1 H26C H -0.0985 0.5196 0.0335 0.185 Uiso 0.560(15) 1 calc PR B 1 C27 C -0.0880(17) 0.4505(18) 0.1226(9) 0.141(8) Uani 0.560(15) 1 d PDU B 1 H27A H -0.0725 0.4627 0.1539 0.212 Uiso 0.560(15) 1 calc PR B 1 H27B H -0.0438 0.4262 0.1054 0.212 Uiso 0.560(15) 1 calc PR B 1 H27C H -0.1290 0.4004 0.1220 0.212 Uiso 0.560(15) 1 calc PR B 1 C26A C -0.1834(15) 0.526(2) 0.1352(9) 0.120(8) Uani 0.440(15) 1 d PDU B 2 H26D H -0.1723 0.5589 0.1641 0.180 Uiso 0.440(15) 1 calc PR B 2 H26E H -0.1892 0.4545 0.1399 0.180 Uiso 0.440(15) 1 calc PR B 2 H26F H -0.2310 0.5537 0.1226 0.180 Uiso 0.440(15) 1 calc PR B 2 C27A C -0.121(2) 0.497(3) 0.0565(8) 0.133(8) Uani 0.440(15) 1 d PDU B 2 H27D H -0.0767 0.5174 0.0383 0.200 Uiso 0.440(15) 1 calc PR B 2 H27E H -0.1686 0.5167 0.0414 0.200 Uiso 0.440(15) 1 calc PR B 2 H27F H -0.1202 0.4241 0.0603 0.200 Uiso 0.440(15) 1 calc PR B 2 P3 P 0.6194(2) 0.6621(3) 0.04809(16) 0.1044(13) Uani 1 1 d DU . . F1 F 0.6720(6) 0.5810(9) 0.0698(5) 0.174(4) Uani 0.603(8) 1 d PDU C 1 F2 F 0.5564(6) 0.5797(8) 0.0376(6) 0.157(4) Uani 0.603(8) 1 d PDU C 1 F3 F 0.5810(8) 0.6844(11) 0.0945(3) 0.160(4) Uani 0.603(8) 1 d PDU C 1 F4 F 0.5656(6) 0.7430(9) 0.0249(5) 0.145(4) Uani 0.603(8) 1 d PDU C 1 F5 F 0.6818(6) 0.7441(8) 0.0560(6) 0.167(4) Uani 0.603(8) 1 d PDU C 1 F6 F 0.6555(8) 0.6393(10) -0.0002(3) 0.152(4) Uani 0.603(8) 1 d PDU C 1 F1A F 0.5695(10) 0.7585(10) 0.0569(7) 0.154(5) Uani 0.397(8) 1 d PDU C 2 F2A F 0.6765(10) 0.7254(13) 0.0188(7) 0.160(5) Uani 0.397(8) 1 d PDU C 2 F3A F 0.5699(10) 0.6369(15) 0.0056(5) 0.160(4) Uani 0.397(8) 1 d PDU C 2 F4A F 0.6694(10) 0.5662(10) 0.0400(7) 0.158(5) Uani 0.397(8) 1 d PDU C 2 F5A F 0.5628(10) 0.6000(13) 0.0789(7) 0.147(5) Uani 0.397(8) 1 d PDU C 2 F6A F 0.6686(10) 0.6875(15) 0.0917(5) 0.145(4) Uani 0.397(8) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0545(3) 0.0732(3) 0.0492(3) -0.0017(2) 0.0087(2) -0.0061(2) Fe 0.0529(10) 0.0727(11) 0.0850(13) -0.0039(10) 0.0084(9) -0.0046(8) P1 0.0572(18) 0.086(2) 0.0551(18) -0.0016(17) 0.0023(14) -0.0023(16) P2 0.0577(18) 0.092(2) 0.0611(19) -0.0009(18) -0.0024(15) -0.0090(17) Cl 0.073(2) 0.130(3) 0.074(2) -0.0021(19) 0.0214(17) -0.0002(19) O1 0.054(5) 0.123(7) 0.057(5) 0.003(5) 0.001(4) -0.002(4) O2 0.066(5) 0.142(8) 0.066(5) -0.008(5) -0.013(5) -0.002(5) C1 0.074(9) 0.071(8) 0.052(7) 0.007(6) 0.004(6) -0.004(6) C2 0.053(7) 0.081(8) 0.054(7) -0.002(6) 0.021(6) -0.013(6) C3 0.059(7) 0.086(8) 0.044(6) -0.009(6) 0.007(6) -0.012(6) C4 0.087(10) 0.102(9) 0.049(7) -0.017(7) -0.002(7) -0.013(8) C5 0.076(10) 0.081(9) 0.129(13) -0.002(9) 0.038(9) 0.000(8) C6 0.079(7) 0.101(7) 0.110(8) -0.007(8) 0.017(7) 0.000(5) C7 0.079(7) 0.101(7) 0.110(8) -0.007(8) 0.017(7) 0.000(5) C8 0.062(8) 0.098(10) 0.104(11) 0.018(8) -0.001(8) 0.018(7) C9 0.074(8) 0.053(7) 0.072(8) -0.001(6) 0.000(7) 0.003(6) C10 0.065(8) 0.059(7) 0.059(7) -0.007(6) 0.000(6) -0.008(6) C11 0.112(16) 0.110(13) 0.17(2) 0.017(14) -0.040(15) -0.052(12) C12 0.20(3) 0.106(15) 0.128(18) -0.041(12) 0.024(19) -0.030(17) C13 0.109(16) 0.064(10) 0.21(3) 0.000(13) 0.055(17) 0.020(9) C14 0.103(14) 0.112(13) 0.113(14) 0.014(10) -0.029(11) 0.004(10) C15 0.080(12) 0.096(11) 0.133(16) 0.016(10) 0.015(10) -0.025(8) C16 0.093(9) 0.107(9) 0.099(10) -0.028(7) -0.020(7) -0.007(8) C17 0.113(16) 0.077(13) 0.135(15) -0.015(12) -0.019(13) -0.006(12) C18 0.093(16) 0.116(17) 0.101(16) -0.019(14) -0.017(13) -0.005(14) C17A 0.130(19) 0.133(18) 0.104(17) -0.049(15) -0.006(14) 0.000(16) C18A 0.115(16) 0.085(14) 0.129(15) -0.016(12) -0.012(13) -0.014(13) C19 0.078(8) 0.107(8) 0.086(9) 0.007(7) -0.009(6) 0.008(7) C20 0.092(16) 0.098(12) 0.112(14) 0.005(11) -0.005(13) 0.005(12) C21 0.140(18) 0.139(17) 0.100(16) 0.028(14) 0.002(14) 0.007(16) C20A 0.091(17) 0.102(13) 0.106(15) 0.014(13) -0.006(14) 0.003(13) C21A 0.082(16) 0.122(17) 0.097(17) 0.030(14) -0.010(13) 0.007(15) C22 0.129(11) 0.094(9) 0.114(11) 0.025(8) -0.015(8) 0.005(7) C23 0.158(13) 0.100(11) 0.131(15) 0.026(12) 0.004(12) -0.011(8) C24 0.128(12) 0.107(13) 0.120(14) 0.002(11) -0.022(10) 0.012(10) C23A 0.145(17) 0.100(16) 0.122(18) 0.024(16) -0.015(15) -0.005(13) C24A 0.13(2) 0.11(2) 0.11(2) 0.029(17) -0.011(15) 0.010(18) C25 0.126(11) 0.128(11) 0.112(10) -0.008(9) -0.029(8) -0.052(9) C26 0.128(16) 0.127(17) 0.116(12) -0.024(12) -0.033(12) -0.044(14) C27 0.148(19) 0.133(15) 0.143(17) 0.002(14) -0.037(15) -0.048(15) C26A 0.131(18) 0.124(19) 0.105(15) 0.006(15) -0.034(11) -0.060(16) C27A 0.148(17) 0.134(18) 0.118(13) -0.015(13) -0.025(13) -0.053(16) P3 0.073(3) 0.109(3) 0.131(3) -0.002(3) 0.022(2) 0.0009(18) F1 0.154(8) 0.163(8) 0.206(10) 0.007(8) -0.018(8) 0.048(6) F2 0.139(7) 0.162(8) 0.169(10) 0.003(8) 0.010(7) -0.055(6) F3 0.158(9) 0.202(10) 0.121(6) -0.009(6) 0.024(6) 0.027(7) F4 0.142(8) 0.153(7) 0.141(9) 0.003(7) 0.002(7) 0.041(6) F5 0.146(7) 0.168(8) 0.186(11) -0.021(8) -0.015(7) -0.049(6) F6 0.147(8) 0.150(9) 0.159(6) -0.030(6) 0.059(6) -0.005(7) F1A 0.144(9) 0.145(7) 0.173(12) -0.005(8) 0.028(8) 0.045(7) F2A 0.151(9) 0.168(10) 0.160(10) 0.005(9) 0.064(8) -0.029(7) F3A 0.157(9) 0.177(10) 0.146(8) -0.009(8) -0.015(7) -0.006(8) F4A 0.158(9) 0.149(7) 0.167(11) -0.010(8) 0.033(8) 0.051(7) F5A 0.128(9) 0.159(10) 0.156(9) 0.006(9) 0.040(8) -0.032(7) F6A 0.121(9) 0.168(10) 0.146(8) -0.007(8) -0.001(7) -0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 1.976(10) . ? Pt P1 2.256(3) . ? Pt P2 2.278(3) . ? Pt Cl 2.363(3) . ? Fe C14 1.997(15) . ? Fe C13 2.020(14) . ? Fe C11 2.023(16) . ? Fe C15 2.026(14) . ? Fe C5 2.027(14) . ? Fe C12 2.028(17) . ? Fe C6 2.054(14) . ? Fe C7 2.059(15) . ? Fe C8 2.061(13) . ? Fe C9 2.110(11) . ? Fe C10 2.163(11) . ? P1 O1 1.666(8) . ? P1 C19 1.804(13) . ? P1 C16 1.827(12) . ? P2 O2 1.605(9) . ? P2 C22 1.775(13) . ? P2 C25 1.815(13) . ? O1 C1 1.400(13) . ? O2 C3 1.350(12) . ? C1 C2 1.311(15) . ? C1 C9 1.490(15) . ? C2 C3 1.443(15) . ? C3 C4 1.362(15) . ? C4 C10 1.394(15) . ? C5 C6 1.342(17) . ? C5 C10 1.429(15) . ? C6 C7 1.409(18) . ? C7 C8 1.369(16) . ? C8 C9 1.373(15) . ? C9 C10 1.447(15) . ? C11 C12 1.31(3) . ? C11 C15 1.39(2) . ? C12 C13 1.40(3) . ? C13 C14 1.35(2) . ? C14 C15 1.38(2) . ? C16 C18 1.473(13) . ? C16 C18A 1.479(13) . ? C16 C17A 1.508(13) . ? C16 C17 1.514(13) . ? C19 C21 1.476(13) . ? C19 C21A 1.481(13) . ? C19 C20A 1.516(13) . ? C19 C20 1.518(13) . ? C22 C24A 1.474(14) . ? C22 C24 1.476(13) . ? C22 C23A 1.517(13) . ? C22 C23 1.518(12) . ? C25 C27 1.469(13) . ? C25 C27A 1.474(14) . ? C25 C26A 1.509(13) . ? C25 C26 1.514(13) . ? P3 F3 1.525(7) . ? P3 F1 1.529(7) . ? P3 F3A 1.530(7) . ? P3 F5 1.531(7) . ? P3 F2A 1.537(7) . ? P3 F4A 1.539(7) . ? P3 F1A 1.546(7) . ? P3 F5A 1.549(7) . ? P3 F6A 1.554(7) . ? P3 F2 1.555(7) . ? P3 F4 1.556(7) . ? P3 F6 1.560(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt P1 81.5(4) . . ? C2 Pt P2 80.6(4) . . ? P1 Pt P2 161.82(12) . . ? C2 Pt Cl 176.5(3) . . ? P1 Pt Cl 97.99(12) . . ? P2 Pt Cl 100.10(12) . . ? C14 Fe C13 39.2(7) . . ? C14 Fe C11 66.5(7) . . ? C13 Fe C11 66.4(8) . . ? C14 Fe C15 40.2(6) . . ? C13 Fe C15 67.2(7) . . ? C11 Fe C15 40.2(7) . . ? C14 Fe C5 106.4(6) . . ? C13 Fe C5 129.0(9) . . ? C11 Fe C5 147.8(9) . . ? C15 Fe C5 113.7(7) . . ? C14 Fe C12 66.0(8) . . ? C13 Fe C12 40.5(8) . . ? C11 Fe C12 37.8(8) . . ? C15 Fe C12 65.9(8) . . ? C5 Fe C12 169.4(10) . . ? C14 Fe C6 125.1(7) . . ? C13 Fe C6 162.8(10) . . ? C11 Fe C6 118.1(8) . . ? C15 Fe C6 104.9(6) . . ? C5 Fe C6 38.4(5) . . ? C12 Fe C6 152.0(10) . . ? C14 Fe C7 157.0(7) . . ? C13 Fe C7 157.1(9) . . ? C11 Fe C7 102.9(7) . . ? C15 Fe C7 118.6(6) . . ? C5 Fe C7 71.1(6) . . ? C12 Fe C7 118.9(9) . . ? C6 Fe C7 40.1(5) . . ? C14 Fe C8 163.1(7) . . ? C13 Fe C8 123.9(8) . . ? C11 Fe C8 111.5(8) . . ? C15 Fe C8 147.2(7) . . ? C5 Fe C8 84.0(6) . . ? C12 Fe C8 101.7(8) . . ? C6 Fe C8 71.3(6) . . ? C7 Fe C8 38.8(5) . . ? C14 Fe C9 131.8(7) . . ? C13 Fe C9 103.7(6) . . ? C11 Fe C9 138.1(9) . . ? C15 Fe C9 170.8(6) . . ? C5 Fe C9 71.0(5) . . ? C12 Fe C9 107.9(8) . . ? C6 Fe C9 83.7(5) . . ? C7 Fe C9 70.1(5) . . ? C8 Fe C9 38.4(4) . . ? C14 Fe C10 108.2(6) . . ? C13 Fe C10 104.6(7) . . ? C11 Fe C10 170.7(8) . . ? C15 Fe C10 139.9(7) . . ? C5 Fe C10 39.7(4) . . ? C12 Fe C10 133.6(9) . . ? C6 Fe C10 71.1(5) . . ? C7 Fe C10 84.7(5) . . ? C8 Fe C10 71.2(5) . . ? C9 Fe C10 39.6(4) . . ? O1 P1 C19 100.4(5) . . ? O1 P1 C16 103.9(6) . . ? C19 P1 C16 109.5(6) . . ? O1 P1 Pt 103.4(3) . . ? C19 P1 Pt 119.7(4) . . ? C16 P1 Pt 116.9(4) . . ? O2 P2 C22 101.9(6) . . ? O2 P2 C25 101.4(6) . . ? C22 P2 C25 109.3(7) . . ? O2 P2 Pt 104.5(3) . . ? C22 P2 Pt 117.6(5) . . ? C25 P2 Pt 119.1(5) . . ? C1 O1 P1 112.5(7) . . ? C3 O2 P2 117.2(8) . . ? C2 C1 O1 122.2(11) . . ? C2 C1 C9 123.9(11) . . ? O1 C1 C9 113.9(10) . . ? C1 C2 C3 119.8(10) . . ? C1 C2 Pt 120.3(9) . . ? C3 C2 Pt 119.9(9) . . ? O2 C3 C4 122.1(11) . . ? O2 C3 C2 117.6(10) . . ? C4 C3 C2 120.3(11) . . ? C3 C4 C10 120.5(11) . . ? C6 C5 C10 124.6(15) . . ? C6 C5 Fe 71.9(9) . . ? C10 C5 Fe 75.3(7) . . ? C5 C6 C7 119.3(14) . . ? C5 C6 Fe 69.7(8) . . ? C7 C6 Fe 70.1(9) . . ? C8 C7 C6 119.3(14) . . ? C8 C7 Fe 70.7(8) . . ? C6 C7 Fe 69.8(9) . . ? C7 C8 C9 121.6(14) . . ? C7 C8 Fe 70.5(9) . . ? C9 C8 Fe 72.7(7) . . ? C8 C9 C10 121.5(11) . . ? C8 C9 C1 125.3(12) . . ? C10 C9 C1 113.1(10) . . ? C8 C9 Fe 68.9(7) . . ? C10 C9 Fe 72.2(6) . . ? C1 C9 Fe 129.4(8) . . ? C4 C10 C5 124.1(12) . . ? C4 C10 C9 122.2(10) . . ? C5 C10 C9 113.4(11) . . ? C4 C10 Fe 132.7(9) . . ? C5 C10 Fe 65.0(7) . . ? C9 C10 Fe 68.2(6) . . ? C12 C11 C15 109(2) . . ? C12 C11 Fe 71.4(11) . . ? C15 C11 Fe 70.0(10) . . ? C11 C12 C13 109(2) . . ? C11 C12 Fe 70.9(11) . . ? C13 C12 Fe 69.5(10) . . ? C14 C13 C12 105.8(18) . . ? C14 C13 Fe 69.5(9) . . ? C12 C13 Fe 70.1(10) . . ? C13 C14 C15 110.0(17) . . ? C13 C14 Fe 71.3(10) . . ? C15 C14 Fe 71.0(9) . . ? C14 C15 C11 105.3(16) . . ? C14 C15 Fe 68.8(9) . . ? C11 C15 Fe 69.8(9) . . ? C18 C16 C18A 109(3) . . ? C18 C16 C17A 98.6(18) . . ? C18A C16 C17A 117.1(12) . . ? C18 C16 C17 117.2(12) . . ? C17A C16 C17 102(3) . . ? C18 C16 P1 113.5(13) . . ? C18A C16 P1 105(2) . . ? C17A C16 P1 113.2(14) . . ? C17 C16 P1 111(2) . . ? C21 C19 C21A 106.1(19) . . ? C21 C19 C20A 89.6(18) . . ? C21A C19 C20A 116.3(11) . . ? C21 C19 C20 116.4(11) . . ? C21A C19 C20 100.8(19) . . ? C21 C19 P1 112.3(13) . . ? C21A C19 P1 115.3(13) . . ? C20A C19 P1 114.0(16) . . ? C20 C19 P1 105.7(14) . . ? C24A C22 C24 82(3) . . ? C24A C22 C23A 116.7(12) . . ? C24 C22 C23A 97(4) . . ? C24A C22 C23 95(3) . . ? C24 C22 C23 116.5(10) . . ? C24A C22 P2 136(3) . . ? C24 C22 P2 112.8(12) . . ? C23A C22 P2 103(3) . . ? C23 C22 P2 112.1(12) . . ? C27 C25 C27A 90(2) . . ? C27 C25 C26A 81.4(19) . . ? C27A C25 C26A 117.4(12) . . ? C27 C25 C26 117.1(11) . . ? C26A C25 C26 113(2) . . ? C27 C25 P2 109.1(14) . . ? C27A C25 P2 121.2(15) . . ? C26A C25 P2 120.1(13) . . ? C26 C25 P2 112.7(15) . . ? F3 P3 F1 91.2(5) . . ? F3 P3 F3A 121.1(7) . . ? F1 P3 F3A 120.3(8) . . ? F3 P3 F5 91.8(5) . . ? F1 P3 F5 91.2(5) . . ? F3A P3 F5 131.0(7) . . ? F3 P3 F2A 131.0(7) . . ? F1 P3 F2A 103.5(9) . . ? F3A P3 F2A 91.2(6) . . ? F3 P3 F4A 121.9(7) . . ? F3A P3 F4A 90.3(6) . . ? F5 P3 F4A 102.3(9) . . ? F2A P3 F4A 90.4(6) . . ? F3 P3 F1A 57.4(7) . . ? F1 P3 F1A 145.6(7) . . ? F3A P3 F1A 90.4(6) . . ? F5 P3 F1A 77.4(9) . . ? F2A P3 F1A 89.8(5) . . ? F4A P3 F1A 179.2(5) . . ? F3 P3 F5A 47.5(7) . . ? F1 P3 F5A 76.1(9) . . ? F3A P3 F5A 90.5(6) . . ? F5 P3 F5A 135.8(7) . . ? F2A P3 F5A 178.3(5) . . ? F4A P3 F5A 90.1(6) . . ? F1A P3 F5A 89.6(5) . . ? F3 P3 F6A 58.1(7) . . ? F1 P3 F6A 59.8(8) . . ? F3A P3 F6A 179.2(5) . . ? F5 P3 F6A 49.6(7) . . ? F2A P3 F6A 89.6(6) . . ? F4A P3 F6A 90.0(6) . . ? F1A P3 F6A 89.3(5) . . ? F5A P3 F6A 88.8(5) . . ? F3 P3 F2 90.5(5) . . ? F1 P3 F2 90.0(5) . . ? F3A P3 F2 46.5(7) . . ? F5 P3 F2 177.4(5) . . ? F2A P3 F2 135.0(7) . . ? F4A P3 F2 77.5(9) . . ? F1A P3 F2 102.8(9) . . ? F5A P3 F2 46.8(6) . . ? F6A P3 F2 132.9(7) . . ? F3 P3 F4 89.9(5) . . ? F1 P3 F4 178.5(5) . . ? F3A P3 F4 58.3(8) . . ? F5 P3 F4 89.7(5) . . ? F2A P3 F4 76.4(9) . . ? F4A P3 F4 145.0(7) . . ? F1A P3 F4 35.8(7) . . ? F5A P3 F4 104.1(9) . . ? F6A P3 F4 121.6(8) . . ? F2 P3 F4 89.1(5) . . ? F3 P3 F6 177.8(5) . . ? F1 P3 F6 90.3(5) . . ? F3A P3 F6 56.8(7) . . ? F5 P3 F6 89.7(5) . . ? F2A P3 F6 50.0(7) . . ? F4A P3 F6 59.2(7) . . ? F1A P3 F6 121.5(7) . . ? F5A P3 F6 131.6(7) . . ? F6A P3 F6 124.0(7) . . ? F2 P3 F6 87.9(5) . . ? F4 P3 F6 88.5(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.162 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.146 #============================================================================== data_compound-6a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H33 Cl Cr Ni O5 P2' _chemical_formula_sum 'C25 H33 Cl Cr Ni O5 P2' _chemical_formula_weight 621.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.728(1) _cell_length_b 10.946(1) _cell_length_c 15.424(1) _cell_angle_alpha 90.00 _cell_angle_beta 109.585(1) _cell_angle_gamma 90.00 _cell_volume 5683.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 837 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Dark Orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7833 _exptl_absorpt_correction_T_max 0.9270 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14470 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.73 _reflns_number_total 5921 _reflns_number_gt 4978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+26.6704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5921 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.153109(12) 0.98462(4) 0.30601(3) 0.02562(12) Uani 1 1 d . . . Cr1 Cr 0.070362(16) 0.56612(5) 0.41512(4) 0.02704(14) Uani 1 1 d . . . Cl1 Cl 0.17253(3) 1.12530(11) 0.23054(8) 0.0528(3) Uani 1 1 d . . . P1 P 0.09286(2) 0.96285(8) 0.21358(6) 0.02440(19) Uani 1 1 d . . . P2 P 0.20939(2) 0.96198(8) 0.41463(6) 0.02549(19) Uani 1 1 d . . . O1 O 0.06957(6) 0.8840(2) 0.27256(15) 0.0256(5) Uani 1 1 d . . . O2 O 0.20162(6) 0.8589(2) 0.48524(15) 0.0271(5) Uani 1 1 d . . . O3 O 0.05271(11) 0.5394(3) 0.2130(2) 0.0606(9) Uani 1 1 d . . . O4 O 0.02625(10) 0.3344(3) 0.4103(3) 0.0593(9) Uani 1 1 d . . . O5 O 0.14269(10) 0.4113(3) 0.4483(3) 0.0644(9) Uani 1 1 d . . . C1 C 0.13556(9) 0.8756(3) 0.3777(2) 0.0230(6) Uani 1 1 d . . . C2 C 0.09653(9) 0.8435(3) 0.3552(2) 0.0226(6) Uani 1 1 d . . . C3 C 0.08108(9) 0.7716(3) 0.4126(2) 0.0230(7) Uani 1 1 d . . . C4 C 0.10914(10) 0.7254(3) 0.4960(2) 0.0234(7) Uani 1 1 d . . . C5 C 0.15031(10) 0.7534(3) 0.5188(2) 0.0240(7) Uani 1 1 d . . . H5 H 0.1692 0.7213 0.5732 0.029 Uiso 1 1 calc R . . C6 C 0.16207(9) 0.8263(3) 0.4620(2) 0.0230(7) Uani 1 1 d . . . C7 C 0.03957(10) 0.7442(3) 0.3907(2) 0.0262(7) Uani 1 1 d . . . H7 H 0.0210 0.7712 0.3340 0.031 Uiso 1 1 calc R . . C8 C 0.02641(10) 0.6785(3) 0.4520(2) 0.0273(7) Uani 1 1 d . . . H8 H -0.0012 0.6656 0.4390 0.033 Uiso 1 1 calc R . . C9 C 0.05403(10) 0.6307(3) 0.5338(2) 0.0290(7) Uani 1 1 d . . . H9 H 0.0449 0.5850 0.5750 0.035 Uiso 1 1 calc R . . C10 C 0.09436(10) 0.6504(3) 0.5538(2) 0.0282(7) Uani 1 1 d . . . H10 H 0.1126 0.6134 0.6070 0.034 Uiso 1 1 calc R . . C11 C 0.08520(11) 0.8653(3) 0.1125(2) 0.0305(8) Uani 1 1 d . . . H11 H 0.0570 0.8367 0.0906 0.037 Uiso 1 1 calc R . . C12 C 0.11229(13) 0.7534(4) 0.1404(3) 0.0461(10) Uani 1 1 d . . . H12A H 0.1064 0.6969 0.0883 0.069 Uiso 1 1 calc R . . H12B H 0.1076 0.7123 0.1923 0.069 Uiso 1 1 calc R . . H12C H 0.1401 0.7793 0.1585 0.069 Uiso 1 1 calc R . . C13 C 0.09256(12) 0.9368(4) 0.0346(3) 0.0391(9) Uani 1 1 d . . . H13A H 0.1180 0.9801 0.0585 0.059 Uiso 1 1 calc R . . H13B H 0.0711 0.9961 0.0093 0.059 Uiso 1 1 calc R . . H13C H 0.0933 0.8802 -0.0140 0.059 Uiso 1 1 calc R . . C14 C 0.06030(10) 1.0941(3) 0.1762(2) 0.0304(8) Uani 1 1 d . . . H14 H 0.0687 1.1381 0.1289 0.036 Uiso 1 1 calc R . . C15 C 0.01679(11) 1.0566(4) 0.1303(3) 0.0394(9) Uani 1 1 d . . . H15A H 0.0068 1.0204 0.1764 0.059 Uiso 1 1 calc R . . H15B H 0.0149 0.9965 0.0818 0.059 Uiso 1 1 calc R . . H15C H 0.0009 1.1287 0.1033 0.059 Uiso 1 1 calc R . . C16 C 0.06575(12) 1.1825(4) 0.2561(3) 0.0427(9) Uani 1 1 d . . . H16A H 0.0485 1.2537 0.2345 0.064 Uiso 1 1 calc R . . H16B H 0.0935 1.2091 0.2802 0.064 Uiso 1 1 calc R . . H16C H 0.0587 1.1413 0.3050 0.064 Uiso 1 1 calc R . . C17 C 0.22922(10) 1.0901(3) 0.4919(2) 0.0306(8) Uani 1 1 d . . . H17 H 0.2379 1.1542 0.4565 0.037 Uiso 1 1 calc R . . C18 C 0.26506(12) 1.0564(4) 0.5756(3) 0.0416(9) Uani 1 1 d . . . H18A H 0.2748 1.1294 0.6133 0.062 Uiso 1 1 calc R . . H18B H 0.2862 1.0235 0.5550 0.062 Uiso 1 1 calc R . . H18C H 0.2572 0.9946 0.6123 0.062 Uiso 1 1 calc R . . C19 C 0.19591(12) 1.1442(4) 0.5214(3) 0.0459(10) Uani 1 1 d . . . H19A H 0.1872 1.0836 0.5574 0.069 Uiso 1 1 calc R . . H19B H 0.1735 1.1666 0.4667 0.069 Uiso 1 1 calc R . . H19C H 0.2057 1.2171 0.5591 0.069 Uiso 1 1 calc R . . C20 C 0.25013(10) 0.8934(3) 0.3859(2) 0.0311(8) Uani 1 1 d . . . H20 H 0.2697 0.8598 0.4437 0.037 Uiso 1 1 calc R . . C21 C 0.27174(11) 0.9866(4) 0.3457(3) 0.0425(10) Uani 1 1 d . . . H21A H 0.2901 0.9440 0.3212 0.064 Uiso 1 1 calc R . . H21B H 0.2866 1.0434 0.3941 0.064 Uiso 1 1 calc R . . H21C H 0.2523 1.0323 0.2961 0.064 Uiso 1 1 calc R . . C22 C 0.23399(12) 0.7869(4) 0.3195(3) 0.0458(10) Uani 1 1 d . . . H22A H 0.2170 0.8187 0.2599 0.069 Uiso 1 1 calc R . . H22B H 0.2185 0.7325 0.3448 0.069 Uiso 1 1 calc R . . H22C H 0.2562 0.7414 0.3113 0.069 Uiso 1 1 calc R . . C23 C 0.05946(12) 0.5489(4) 0.2895(3) 0.0387(9) Uani 1 1 d . . . C24 C 0.04312(11) 0.4251(4) 0.4118(3) 0.0380(9) Uani 1 1 d . . . C25 C 0.11511(12) 0.4718(4) 0.4355(3) 0.0397(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0220(2) 0.0275(2) 0.0268(2) 0.00762(18) 0.00745(17) 0.00026(17) Cr1 0.0265(3) 0.0264(3) 0.0301(3) -0.0010(2) 0.0121(2) -0.0017(2) Cl1 0.0360(5) 0.0636(7) 0.0541(6) 0.0340(5) 0.0089(4) -0.0086(5) P1 0.0223(4) 0.0271(5) 0.0236(4) 0.0052(3) 0.0074(3) 0.0011(3) P2 0.0204(4) 0.0268(5) 0.0284(4) 0.0040(3) 0.0070(3) -0.0003(3) O1 0.0192(11) 0.0310(13) 0.0248(11) 0.0078(10) 0.0049(9) 0.0004(10) O2 0.0215(11) 0.0300(13) 0.0270(12) 0.0061(10) 0.0042(9) -0.0014(10) O3 0.078(2) 0.062(2) 0.0392(18) -0.0158(15) 0.0165(16) 0.0011(18) O4 0.065(2) 0.0384(18) 0.093(3) -0.0161(17) 0.051(2) -0.0194(16) O5 0.0457(19) 0.055(2) 0.093(3) 0.0008(19) 0.0235(18) 0.0159(17) C1 0.0246(16) 0.0214(16) 0.0230(15) 0.0006(13) 0.0078(12) -0.0001(13) C2 0.0231(16) 0.0226(16) 0.0211(15) -0.0005(12) 0.0062(12) 0.0027(13) C3 0.0244(16) 0.0216(16) 0.0239(16) -0.0004(13) 0.0095(13) 0.0035(13) C4 0.0286(17) 0.0211(16) 0.0216(15) -0.0022(13) 0.0098(13) -0.0008(13) C5 0.0267(16) 0.0232(17) 0.0197(15) 0.0011(12) 0.0047(12) 0.0036(13) C6 0.0197(15) 0.0221(16) 0.0275(16) 0.0003(13) 0.0081(12) 0.0029(13) C7 0.0246(16) 0.0269(18) 0.0271(17) 0.0002(14) 0.0086(13) 0.0022(14) C8 0.0259(17) 0.0257(17) 0.0335(18) -0.0014(14) 0.0144(14) 0.0003(14) C9 0.0342(19) 0.0291(19) 0.0284(17) -0.0026(14) 0.0169(14) -0.0026(15) C10 0.0334(18) 0.0289(18) 0.0226(16) 0.0031(14) 0.0098(14) 0.0014(15) C11 0.0293(18) 0.032(2) 0.0305(18) -0.0011(15) 0.0110(14) -0.0034(15) C12 0.051(3) 0.041(2) 0.047(2) 0.0001(19) 0.018(2) 0.008(2) C13 0.039(2) 0.051(2) 0.0304(19) 0.0021(17) 0.0161(16) -0.0038(19) C14 0.0302(18) 0.0283(19) 0.0329(18) 0.0080(15) 0.0108(14) 0.0040(15) C15 0.0288(19) 0.045(2) 0.040(2) 0.0045(18) 0.0063(16) 0.0121(17) C16 0.042(2) 0.034(2) 0.049(2) -0.0023(18) 0.0124(18) 0.0052(18) C17 0.0295(18) 0.0292(19) 0.0348(19) -0.0005(15) 0.0130(15) -0.0060(15) C18 0.037(2) 0.044(2) 0.039(2) -0.0082(18) 0.0067(17) -0.0064(18) C19 0.042(2) 0.041(2) 0.057(3) -0.009(2) 0.020(2) 0.0024(19) C20 0.0239(17) 0.037(2) 0.0319(18) 0.0047(15) 0.0083(14) 0.0058(15) C21 0.031(2) 0.053(3) 0.048(2) 0.012(2) 0.0204(18) 0.0035(18) C22 0.041(2) 0.045(2) 0.052(3) -0.008(2) 0.0167(19) 0.0085(19) C23 0.042(2) 0.036(2) 0.039(2) 0.0017(17) 0.0160(17) 0.0018(17) C24 0.034(2) 0.038(2) 0.048(2) -0.0046(18) 0.0217(17) -0.0026(17) C25 0.037(2) 0.037(2) 0.046(2) -0.0039(18) 0.0147(17) -0.0038(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.872(3) . ? Ni1 P2 2.1570(9) . ? Ni1 P1 2.1599(9) . ? Ni1 Cl1 2.1793(10) . ? Cr1 C24 1.817(4) . ? Cr1 C25 1.840(4) . ? Cr1 C23 1.853(4) . ? Cr1 C7 2.208(3) . ? Cr1 C8 2.214(3) . ? Cr1 C9 2.215(3) . ? Cr1 C10 2.221(3) . ? Cr1 C3 2.285(3) . ? Cr1 C4 2.314(3) . ? P1 O1 1.665(2) . ? P1 C14 1.817(4) . ? P1 C11 1.833(4) . ? P2 O2 1.655(2) . ? P2 C20 1.820(4) . ? P2 C17 1.824(4) . ? O1 C2 1.387(4) . ? O2 C6 1.383(4) . ? O3 C23 1.128(5) . ? O4 C24 1.158(5) . ? O5 C25 1.148(5) . ? C1 C2 1.365(4) . ? C1 C6 1.433(4) . ? C2 C3 1.427(4) . ? C3 C4 1.433(4) . ? C3 C7 1.438(4) . ? C4 C5 1.426(4) . ? C4 C10 1.436(4) . ? C5 C6 1.352(5) . ? C5 H5 0.9500 . ? C7 C8 1.389(5) . ? C7 H7 0.9500 . ? C8 C9 1.416(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C13 1.529(5) . ? C11 C12 1.531(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.526(5) . ? C14 C15 1.533(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.528(5) . ? C17 C19 1.528(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.530(5) . ? C20 C22 1.531(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 P2 82.97(10) . . ? C1 Ni1 P1 82.10(10) . . ? P2 Ni1 P1 164.42(4) . . ? C1 Ni1 Cl1 174.59(11) . . ? P2 Ni1 Cl1 96.62(4) . . ? P1 Ni1 Cl1 98.66(4) . . ? C24 Cr1 C25 87.41(18) . . ? C24 Cr1 C23 87.80(18) . . ? C25 Cr1 C23 89.30(18) . . ? C24 Cr1 C7 120.92(15) . . ? C25 Cr1 C7 151.59(16) . . ? C23 Cr1 C7 89.62(15) . . ? C24 Cr1 C8 93.43(15) . . ? C25 Cr1 C8 156.73(16) . . ? C23 Cr1 C8 113.97(16) . . ? C7 Cr1 C8 36.61(12) . . ? C24 Cr1 C9 90.41(15) . . ? C25 Cr1 C9 119.51(16) . . ? C23 Cr1 C9 151.03(16) . . ? C7 Cr1 C9 66.72(13) . . ? C8 Cr1 C9 37.29(13) . . ? C24 Cr1 C10 114.19(16) . . ? C25 Cr1 C10 92.04(16) . . ? C23 Cr1 C10 158.00(16) . . ? C7 Cr1 C10 78.87(13) . . ? C8 Cr1 C10 66.41(13) . . ? C9 Cr1 C10 36.40(12) . . ? C24 Cr1 C3 158.07(15) . . ? C25 Cr1 C3 114.49(15) . . ? C23 Cr1 C3 93.45(15) . . ? C7 Cr1 C3 37.29(11) . . ? C8 Cr1 C3 66.07(12) . . ? C9 Cr1 C3 77.98(12) . . ? C10 Cr1 C3 66.09(12) . . ? C24 Cr1 C4 150.84(15) . . ? C25 Cr1 C4 90.10(15) . . ? C23 Cr1 C4 121.23(15) . . ? C7 Cr1 C4 66.48(12) . . ? C8 Cr1 C4 77.92(12) . . ? C9 Cr1 C4 65.78(12) . . ? C10 Cr1 C4 36.85(11) . . ? C3 Cr1 C4 36.30(11) . . ? O1 P1 C14 101.49(14) . . ? O1 P1 C11 101.73(14) . . ? C14 P1 C11 107.08(17) . . ? O1 P1 Ni1 105.46(8) . . ? C14 P1 Ni1 120.84(12) . . ? C11 P1 Ni1 117.21(12) . . ? O2 P2 C20 101.73(15) . . ? O2 P2 C17 102.04(15) . . ? C20 P2 C17 108.03(17) . . ? O2 P2 Ni1 105.73(9) . . ? C20 P2 Ni1 118.13(12) . . ? C17 P2 Ni1 118.44(12) . . ? C2 O1 P1 110.30(19) . . ? C6 O2 P2 112.81(19) . . ? C2 C1 C6 116.2(3) . . ? C2 C1 Ni1 122.0(2) . . ? C6 C1 Ni1 121.7(2) . . ? C1 C2 O1 119.2(3) . . ? C1 C2 C3 123.9(3) . . ? O1 C2 C3 116.9(3) . . ? C2 C3 C4 116.9(3) . . ? C2 C3 C7 123.5(3) . . ? C4 C3 C7 119.6(3) . . ? C2 C3 Cr1 130.9(2) . . ? C4 C3 Cr1 72.99(18) . . ? C7 C3 Cr1 68.46(19) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 C10 122.2(3) . . ? C3 C4 C10 117.9(3) . . ? C5 C4 Cr1 132.6(2) . . ? C3 C4 Cr1 70.71(18) . . ? C10 C4 Cr1 68.05(18) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 O2 119.8(3) . . ? C5 C6 C1 123.8(3) . . ? O2 C6 C1 116.4(3) . . ? C8 C7 C3 120.4(3) . . ? C8 C7 Cr1 71.9(2) . . ? C3 C7 Cr1 74.25(19) . . ? C8 C7 H7 119.8 . . ? C3 C7 H7 119.8 . . ? Cr1 C7 H7 125.8 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 Cr1 71.45(19) . . ? C9 C8 Cr1 71.39(19) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? Cr1 C8 H8 129.8 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 Cr1 72.05(19) . . ? C8 C9 Cr1 71.32(19) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? Cr1 C9 H9 129.1 . . ? C9 C10 C4 121.4(3) . . ? C9 C10 Cr1 71.6(2) . . ? C4 C10 Cr1 75.11(18) . . ? C9 C10 H10 119.3 . . ? C4 C10 H10 119.3 . . ? Cr1 C10 H10 125.9 . . ? C13 C11 C12 111.9(3) . . ? C13 C11 P1 110.8(3) . . ? C12 C11 P1 109.1(3) . . ? C13 C11 H11 108.4 . . ? C12 C11 H11 108.4 . . ? P1 C11 H11 108.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 112.2(3) . . ? C16 C14 P1 110.5(3) . . ? C15 C14 P1 112.1(3) . . ? C16 C14 H14 107.2 . . ? C15 C14 H14 107.2 . . ? P1 C14 H14 107.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 111.0(3) . . ? C18 C17 P2 113.5(3) . . ? C19 C17 P2 108.8(3) . . ? C18 C17 H17 107.8 . . ? C19 C17 H17 107.8 . . ? P2 C17 H17 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.4(3) . . ? C21 C20 P2 112.1(3) . . ? C22 C20 P2 108.9(3) . . ? C21 C20 H20 108.1 . . ? C22 C20 H20 108.1 . . ? P2 C20 H20 108.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 Cr1 179.4(4) . . ? O4 C24 Cr1 179.0(4) . . ? O5 C25 Cr1 178.9(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.481 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.081 #============================================================================== data_compound-6b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H33 Cl Cr O5 P2 Pd' _chemical_formula_sum 'C25 H33 Cl Cr O5 P2 Pd' _chemical_formula_weight 669.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.488(1) _cell_length_b 13.505(1) _cell_length_c 18.355(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2847.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 2526 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6345 _exptl_absorpt_correction_T_max 0.7368 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21336 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8106 _reflns_number_gt 8001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+1.3705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(12) _refine_ls_number_reflns 8106 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.840885(10) 0.600442(9) 0.182201(6) 0.01782(3) Uani 1 1 d . . . Cr1 Cr 1.05999(2) 0.34930(2) -0.053022(15) 0.02073(6) Uani 1 1 d . . . Cl1 Cl 0.83058(5) 0.71623(4) 0.27781(2) 0.02946(9) Uani 1 1 d . . . P1 P 0.98720(4) 0.50318(3) 0.22550(2) 0.01975(8) Uani 1 1 d . . . P2 P 0.69447(4) 0.65762(3) 0.11057(2) 0.01839(8) Uani 1 1 d . . . O1 O 1.00410(11) 0.41690(10) 0.16224(6) 0.0231(3) Uani 1 1 d . . . O2 O 0.70329(10) 0.59095(10) 0.03500(7) 0.0219(2) Uani 1 1 d . . . O3 O 1.01921(16) 0.52531(12) -0.14949(9) 0.0402(4) Uani 1 1 d . . . O4 O 1.26273(15) 0.44926(14) 0.01856(12) 0.0455(4) Uani 1 1 d . . . O5 O 1.23489(17) 0.26783(15) -0.15775(10) 0.0499(5) Uani 1 1 d . . . C1 C 0.85333(14) 0.50499(12) 0.10058(9) 0.0186(3) Uani 1 1 d . . . C2 C 0.93150(15) 0.42829(13) 0.10308(9) 0.0187(3) Uani 1 1 d . . . C3 C 0.94023(15) 0.35549(13) 0.04690(9) 0.0191(3) Uani 1 1 d . . . C4 C 0.86767(14) 0.36865(13) -0.01576(9) 0.0197(3) Uani 1 1 d . . . C5 C 0.78970(14) 0.45009(13) -0.02026(9) 0.0201(3) Uani 1 1 d . . . H5 H 0.7435 0.4601 -0.0625 0.024 Uiso 1 1 calc R . . C6 C 0.78251(14) 0.51372(13) 0.03743(9) 0.0194(3) Uani 1 1 d . . . C7 C 1.01827(16) 0.27288(13) 0.05048(10) 0.0231(3) Uani 1 1 d . . . H7 H 1.0692 0.2658 0.0909 0.028 Uiso 1 1 calc R . . C8 C 1.01956(18) 0.20267(14) -0.00547(10) 0.0263(4) Uani 1 1 d . . . H8 H 1.0674 0.1456 -0.0014 0.032 Uiso 1 1 calc R . . C9 C 0.94985(18) 0.21637(14) -0.06815(10) 0.0267(4) Uani 1 1 d . . . H9 H 0.9522 0.1688 -0.1063 0.032 Uiso 1 1 calc R . . C10 C 0.87780(16) 0.29890(14) -0.07454(10) 0.0236(3) Uani 1 1 d . . . H10 H 0.8350 0.3092 -0.1182 0.028 Uiso 1 1 calc R . . C11 C 0.96228(16) 0.42993(14) 0.30736(10) 0.0249(3) Uani 1 1 d . . . H11 H 1.0182 0.3732 0.3080 0.030 Uiso 1 1 calc R . . C12 C 0.8378(2) 0.38928(17) 0.30605(12) 0.0375(4) Uani 1 1 d . . . H12A H 0.8249 0.3477 0.3491 0.056 Uiso 1 1 calc R . . H12B H 0.8264 0.3496 0.2619 0.056 Uiso 1 1 calc R . . H12C H 0.7824 0.4445 0.3063 0.056 Uiso 1 1 calc R . . C13 C 0.98285(18) 0.49409(17) 0.37511(10) 0.0307(4) Uani 1 1 d . . . H13A H 0.9372 0.5552 0.3712 0.046 Uiso 1 1 calc R . . H13B H 1.0657 0.5106 0.3788 0.046 Uiso 1 1 calc R . . H13C H 0.9588 0.4575 0.4187 0.046 Uiso 1 1 calc R . . C14 C 1.13132(16) 0.55826(15) 0.23348(10) 0.0255(4) Uani 1 1 d . . . H14 H 1.1277 0.6086 0.2734 0.031 Uiso 1 1 calc R . . C15 C 1.1600(2) 0.61303(18) 0.16323(12) 0.0387(5) Uani 1 1 d . . . H15A H 1.2317 0.6514 0.1699 0.058 Uiso 1 1 calc R . . H15B H 1.0959 0.6579 0.1509 0.058 Uiso 1 1 calc R . . H15C H 1.1710 0.5651 0.1237 0.058 Uiso 1 1 calc R . . C16 C 1.22608(18) 0.48361(19) 0.25379(14) 0.0378(5) Uani 1 1 d . . . H16A H 1.2306 0.4322 0.2162 0.057 Uiso 1 1 calc R . . H16B H 1.2072 0.4531 0.3008 0.057 Uiso 1 1 calc R . . H16C H 1.3012 0.5177 0.2574 0.057 Uiso 1 1 calc R . . C17 C 0.54662(16) 0.63193(16) 0.14109(11) 0.0276(4) Uani 1 1 d . . . H17 H 0.4920 0.6444 0.0997 0.033 Uiso 1 1 calc R . . C18 C 0.51370(18) 0.70035(18) 0.20419(12) 0.0352(5) Uani 1 1 d . . . H18A H 0.4340 0.6857 0.2200 0.053 Uiso 1 1 calc R . . H18B H 0.5185 0.7694 0.1881 0.053 Uiso 1 1 calc R . . H18C H 0.5675 0.6898 0.2449 0.053 Uiso 1 1 calc R . . C19 C 0.5386(2) 0.52273(19) 0.16247(17) 0.0488(7) Uani 1 1 d . . . H19A H 0.5885 0.5103 0.2048 0.073 Uiso 1 1 calc R . . H19B H 0.5644 0.4815 0.1216 0.073 Uiso 1 1 calc R . . H19C H 0.4578 0.5064 0.1747 0.073 Uiso 1 1 calc R . . C20 C 0.69692(16) 0.78391(14) 0.07504(10) 0.0231(3) Uani 1 1 d . . . H20 H 0.6905 0.8298 0.1176 0.028 Uiso 1 1 calc R . . C21 C 0.81521(19) 0.80231(18) 0.03939(15) 0.0393(5) Uani 1 1 d . . . H21A H 0.8228 0.7605 -0.0040 0.059 Uiso 1 1 calc R . . H21B H 0.8773 0.7861 0.0740 0.059 Uiso 1 1 calc R . . H21C H 0.8213 0.8721 0.0253 0.059 Uiso 1 1 calc R . . C22 C 0.59590(19) 0.80709(17) 0.02373(12) 0.0328(4) Uani 1 1 d . . . H22A H 0.6041 0.8747 0.0051 0.049 Uiso 1 1 calc R . . H22B H 0.5222 0.8011 0.0502 0.049 Uiso 1 1 calc R . . H22C H 0.5966 0.7603 -0.0171 0.049 Uiso 1 1 calc R . . C23 C 1.03664(17) 0.45748(15) -0.11272(11) 0.0275(4) Uani 1 1 d . . . C24 C 1.18367(17) 0.41161(15) -0.00828(11) 0.0294(4) Uani 1 1 d . . . C25 C 1.1669(2) 0.29887(16) -0.11751(11) 0.0317(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01947(5) 0.01866(5) 0.01534(5) -0.00297(4) -0.00269(4) 0.00258(4) Cr1 0.02296(12) 0.02047(13) 0.01876(12) -0.00097(10) 0.00166(10) 0.00393(10) Cl1 0.0353(2) 0.0291(2) 0.02403(19) -0.01090(16) -0.00184(18) 0.00074(19) P1 0.02178(19) 0.0219(2) 0.01552(18) -0.00221(16) -0.00382(15) 0.00331(16) P2 0.01712(17) 0.01981(19) 0.01826(19) -0.00244(15) -0.00132(14) 0.00229(15) O1 0.0259(6) 0.0256(6) 0.0178(5) -0.0038(5) -0.0069(5) 0.0078(5) O2 0.0213(5) 0.0249(6) 0.0194(5) -0.0045(5) -0.0044(4) 0.0062(5) O3 0.0504(9) 0.0345(8) 0.0356(8) 0.0116(7) 0.0022(7) 0.0047(7) O4 0.0334(8) 0.0388(9) 0.0643(12) -0.0028(9) -0.0122(8) -0.0035(7) O5 0.0510(10) 0.0516(11) 0.0470(10) -0.0056(9) 0.0215(8) 0.0153(9) C1 0.0208(7) 0.0196(7) 0.0154(7) -0.0039(5) -0.0016(6) 0.0025(6) C2 0.0213(7) 0.0199(7) 0.0147(7) -0.0010(6) -0.0024(6) 0.0021(6) C3 0.0222(7) 0.0185(7) 0.0166(7) -0.0002(6) 0.0007(6) 0.0017(6) C4 0.0204(7) 0.0204(7) 0.0182(7) -0.0014(6) 0.0002(6) 0.0003(6) C5 0.0199(7) 0.0239(8) 0.0166(7) -0.0029(6) -0.0020(6) 0.0013(6) C6 0.0179(7) 0.0208(7) 0.0194(8) -0.0011(6) -0.0012(6) 0.0029(6) C7 0.0289(8) 0.0203(8) 0.0201(7) 0.0005(6) -0.0009(7) 0.0050(6) C8 0.0365(9) 0.0191(8) 0.0231(8) -0.0015(6) 0.0024(7) 0.0060(7) C9 0.0341(9) 0.0227(8) 0.0232(8) -0.0069(7) 0.0004(7) 0.0011(7) C10 0.0273(8) 0.0230(8) 0.0204(8) -0.0056(6) -0.0017(6) 0.0004(7) C11 0.0305(8) 0.0250(8) 0.0192(8) 0.0019(6) -0.0014(6) 0.0048(6) C12 0.0437(11) 0.0354(10) 0.0335(10) 0.0037(8) 0.0007(9) -0.0114(10) C13 0.0331(9) 0.0412(11) 0.0179(8) -0.0007(8) -0.0006(7) 0.0041(9) C14 0.0244(8) 0.0284(9) 0.0238(9) -0.0022(7) -0.0057(6) 0.0012(7) C15 0.0393(10) 0.0393(11) 0.0375(11) 0.0098(9) -0.0012(9) -0.0071(10) C16 0.0238(9) 0.0433(12) 0.0463(13) 0.0053(10) -0.0046(8) 0.0060(9) C17 0.0211(8) 0.0321(10) 0.0296(9) -0.0055(8) 0.0023(7) -0.0027(7) C18 0.0278(9) 0.0430(12) 0.0346(10) -0.0088(9) 0.0100(8) 0.0010(9) C19 0.0476(13) 0.0332(12) 0.0655(18) -0.0047(11) 0.0253(12) -0.0141(10) C20 0.0231(7) 0.0218(8) 0.0244(8) 0.0005(6) -0.0014(6) 0.0031(6) C21 0.0304(10) 0.0340(11) 0.0535(14) 0.0104(10) 0.0062(9) -0.0031(8) C22 0.0355(10) 0.0320(10) 0.0309(10) 0.0040(8) -0.0094(8) 0.0070(8) C23 0.0297(9) 0.0271(9) 0.0256(9) 0.0008(7) 0.0035(7) 0.0025(7) C24 0.0278(9) 0.0259(9) 0.0346(10) 0.0011(8) -0.0003(7) 0.0049(7) C25 0.0346(9) 0.0323(10) 0.0281(9) -0.0005(7) 0.0055(8) 0.0057(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.9816(16) . ? Pd1 P2 2.2702(5) . ? Pd1 P1 2.2765(5) . ? Pd1 Cl1 2.3535(4) . ? Cr1 C25 1.837(2) . ? Cr1 C24 1.844(2) . ? Cr1 C23 1.846(2) . ? Cr1 C8 2.213(2) . ? Cr1 C9 2.214(2) . ? Cr1 C7 2.2145(18) . ? Cr1 C10 2.2361(19) . ? Cr1 C3 2.2942(17) . ? Cr1 C4 2.3275(16) . ? P1 O1 1.6565(13) . ? P1 C14 1.8210(19) . ? P1 C11 1.8216(19) . ? P2 O2 1.6569(13) . ? P2 C17 1.8219(19) . ? P2 C20 1.8263(19) . ? O1 C2 1.3778(19) . ? O2 C6 1.385(2) . ? O3 C23 1.155(2) . ? O4 C24 1.152(3) . ? O5 C25 1.154(3) . ? C1 C2 1.372(2) . ? C1 C6 1.421(2) . ? C2 C3 1.428(2) . ? C3 C4 1.432(2) . ? C3 C7 1.433(2) . ? C4 C5 1.421(2) . ? C4 C10 1.437(2) . ? C5 C6 1.366(2) . ? C5 H5 0.9500 . ? C7 C8 1.398(2) . ? C7 H7 0.9500 . ? C8 C9 1.414(3) . ? C8 H8 0.9500 . ? C9 C10 1.393(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.532(3) . ? C11 C13 1.534(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.523(3) . ? C14 C16 1.530(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.529(3) . ? C17 C18 1.529(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.527(3) . ? C20 C21 1.529(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P2 80.61(5) . . ? C1 Pd1 P1 80.52(5) . . ? P2 Pd1 P1 160.996(17) . . ? C1 Pd1 Cl1 178.40(5) . . ? P2 Pd1 Cl1 99.707(18) . . ? P1 Pd1 Cl1 99.215(18) . . ? C25 Cr1 C24 86.62(10) . . ? C25 Cr1 C23 90.46(9) . . ? C24 Cr1 C23 90.87(9) . . ? C25 Cr1 C8 93.59(8) . . ? C24 Cr1 C8 113.22(8) . . ? C23 Cr1 C8 155.75(8) . . ? C25 Cr1 C9 90.03(9) . . ? C24 Cr1 C9 150.02(8) . . ? C23 Cr1 C9 118.97(8) . . ? C8 Cr1 C9 37.25(7) . . ? C25 Cr1 C7 121.65(8) . . ? C24 Cr1 C7 89.85(8) . . ? C23 Cr1 C7 147.86(8) . . ? C8 Cr1 C7 36.80(6) . . ? C9 Cr1 C7 66.79(7) . . ? C25 Cr1 C10 113.52(9) . . ? C24 Cr1 C10 159.83(8) . . ? C23 Cr1 C10 90.00(8) . . ? C8 Cr1 C10 66.48(7) . . ? C9 Cr1 C10 36.49(7) . . ? C7 Cr1 C10 78.88(7) . . ? C25 Cr1 C3 158.39(8) . . ? C24 Cr1 C3 95.13(8) . . ? C23 Cr1 C3 111.02(7) . . ? C8 Cr1 C3 65.89(6) . . ? C9 Cr1 C3 77.70(7) . . ? C7 Cr1 C3 37.00(6) . . ? C10 Cr1 C3 65.86(6) . . ? C25 Cr1 C4 149.96(8) . . ? C24 Cr1 C4 123.31(7) . . ? C23 Cr1 C4 87.00(7) . . ? C8 Cr1 C4 77.61(7) . . ? C9 Cr1 C4 65.50(7) . . ? C7 Cr1 C4 66.10(6) . . ? C10 Cr1 C4 36.64(6) . . ? C3 Cr1 C4 36.08(6) . . ? O1 P1 C14 103.72(8) . . ? O1 P1 C11 102.39(8) . . ? C14 P1 C11 107.37(9) . . ? O1 P1 Pd1 104.34(5) . . ? C14 P1 Pd1 117.63(7) . . ? C11 P1 Pd1 119.03(6) . . ? O2 P2 C17 102.18(8) . . ? O2 P2 C20 101.98(8) . . ? C17 P2 C20 107.58(9) . . ? O2 P2 Pd1 104.76(5) . . ? C17 P2 Pd1 116.61(7) . . ? C20 P2 Pd1 120.87(6) . . ? C2 O1 P1 113.77(11) . . ? C6 O2 P2 114.98(10) . . ? C2 C1 C6 117.70(15) . . ? C2 C1 Pd1 120.88(12) . . ? C6 C1 Pd1 121.42(12) . . ? C1 C2 O1 120.46(15) . . ? C1 C2 C3 122.80(15) . . ? O1 C2 C3 116.72(14) . . ? C2 C3 C4 116.98(15) . . ? C2 C3 C7 123.16(15) . . ? C4 C3 C7 119.86(15) . . ? C2 C3 Cr1 130.12(12) . . ? C4 C3 Cr1 73.23(9) . . ? C7 C3 Cr1 68.47(10) . . ? C5 C4 C3 120.66(15) . . ? C5 C4 C10 120.99(15) . . ? C3 C4 C10 118.34(15) . . ? C5 C4 Cr1 131.93(13) . . ? C3 C4 Cr1 70.69(9) . . ? C10 C4 Cr1 68.22(10) . . ? C6 C5 C4 118.68(15) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 O2 119.24(15) . . ? C5 C6 C1 123.05(15) . . ? O2 C6 C1 117.72(15) . . ? C8 C7 C3 120.08(17) . . ? C8 C7 Cr1 71.56(11) . . ? C3 C7 Cr1 74.53(10) . . ? C8 C7 H7 120.0 . . ? C3 C7 H7 120.0 . . ? Cr1 C7 H7 125.7 . . ? C7 C8 C9 120.20(17) . . ? C7 C8 Cr1 71.64(11) . . ? C9 C8 Cr1 71.39(11) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? Cr1 C8 H8 129.5 . . ? C10 C9 C8 120.65(17) . . ? C10 C9 Cr1 72.63(11) . . ? C8 C9 Cr1 71.36(11) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? Cr1 C9 H9 128.6 . . ? C9 C10 C4 120.61(17) . . ? C9 C10 Cr1 70.89(11) . . ? C4 C10 Cr1 75.14(10) . . ? C9 C10 H10 119.7 . . ? C4 C10 H10 119.7 . . ? Cr1 C10 H10 126.1 . . ? C12 C11 C13 111.04(16) . . ? C12 C11 P1 109.16(13) . . ? C13 C11 P1 109.74(14) . . ? C12 C11 H11 109.0 . . ? C13 C11 H11 109.0 . . ? P1 C11 H11 109.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 111.86(18) . . ? C15 C14 P1 109.11(14) . . ? C16 C14 P1 113.42(15) . . ? C15 C14 H14 107.4 . . ? C16 C14 H14 107.4 . . ? P1 C14 H14 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 111.94(19) . . ? C19 C17 P2 108.59(15) . . ? C18 C17 P2 110.39(14) . . ? C19 C17 H17 108.6 . . ? C18 C17 H17 108.6 . . ? P2 C17 H17 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 112.23(17) . . ? C22 C20 P2 113.58(14) . . ? C21 C20 P2 108.56(14) . . ? C22 C20 H20 107.4 . . ? C21 C20 H20 107.4 . . ? P2 C20 H20 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 Cr1 178.30(19) . . ? O4 C24 Cr1 178.3(2) . . ? O5 C25 Cr1 179.3(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.352 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.053 #============================================================================== data_compound-6c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H33 Cl Cr O5 P2 Pt' _chemical_formula_sum 'C25 H33 Cl Cr O5 P2 Pt' _chemical_formula_weight 757.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.5738(10) _cell_length_b 13.6509(12) _cell_length_c 18.4648(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2917.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9665 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.38 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 5.395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3556 _exptl_absorpt_correction_T_max 0.4862 _exptl_absorpt_process_details 'sadabs, Sheldrick, G. M. (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX AXS CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_reflns_number 32274 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.38 _reflns_number_total 5357 _reflns_number_gt 5104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _solved_by 'Simon Hernandez-Ortega' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(4) _refine_ls_number_reflns 5357 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 1.06059(6) 0.85004(5) -0.05267(4) 0.04479(17) Uani 1 1 d . . . Pt Pt 0.842526(13) 1.096175(11) 0.181868(8) 0.03709(5) Uani 1 1 d . . . Cl Cl 0.83239(13) 1.21116(9) 0.27723(6) 0.0607(3) Uani 1 1 d . . . P1 P 0.69859(9) 1.15376(8) 0.11122(6) 0.0385(2) Uani 1 1 d . . . P2 P 0.98702(10) 1.00088(8) 0.22526(5) 0.0408(3) Uani 1 1 d . . . O1 O 0.7069(2) 1.0871(2) 0.03670(14) 0.0443(7) Uani 1 1 d . . . O2 O 1.0038(2) 0.9161(2) 0.16235(13) 0.0449(7) Uani 1 1 d . . . O3 O 1.0218(4) 1.0239(3) -0.1476(2) 0.0857(13) Uani 1 1 d . . . O4 O 1.2328(4) 0.7712(4) -0.1573(2) 0.1041(16) Uani 1 1 d . . . O5 O 1.2613(4) 0.9502(3) 0.0161(3) 0.0941(14) Uani 1 1 d . . . C1 C 0.9323(3) 0.9261(3) 0.1028(2) 0.0366(9) Uani 1 1 d . . . C2 C 0.8551(4) 1.0026(3) 0.1012(2) 0.0369(9) Uani 1 1 d . . . C3 C 0.7850(3) 1.0106(3) 0.0383(2) 0.0378(9) Uani 1 1 d . . . C4 C 0.7922(4) 0.9477(3) -0.0191(2) 0.0406(9) Uani 1 1 d . . . H4 H 0.7469 0.9571 -0.0601 0.049 Uiso 1 1 calc R . . C5 C 0.8800(4) 0.7994(3) -0.0729(2) 0.0485(11) Uani 1 1 d . . . H5 H 0.8374 0.8090 -0.1150 0.058 Uiso 1 1 calc R . . C6 C 0.9521(5) 0.7191(3) -0.0676(2) 0.0555(12) Uani 1 1 d . . . H6 H 0.9549 0.6738 -0.1052 0.067 Uiso 1 1 calc R . . C7 C 1.0214(5) 0.7052(3) -0.0056(2) 0.0550(12) Uani 1 1 d . . . H7 H 1.0682 0.6501 -0.0018 0.066 Uiso 1 1 calc R . . C8 C 1.0195(4) 0.7741(3) 0.0496(2) 0.0474(10) Uani 1 1 d . . . H8 H 1.0693 0.7671 0.0888 0.057 Uiso 1 1 calc R . . C9 C 0.9430(4) 0.8552(3) 0.0473(2) 0.0399(9) Uani 1 1 d . . . C10 C 0.8698(3) 0.8681(3) -0.0147(2) 0.0394(10) Uani 1 1 d . . . C11 C 1.0377(5) 0.9561(4) -0.1117(3) 0.0583(13) Uani 1 1 d . . . C12 C 1.1649(5) 0.8006(4) -0.1172(3) 0.0662(14) Uani 1 1 d . . . C13 C 1.1831(4) 0.9120(4) -0.0097(3) 0.0600(12) Uani 1 1 d . . . C14 C 0.7037(4) 1.2784(4) 0.0754(2) 0.0496(11) Uani 1 1 d . . . H14 H 0.6965 1.3235 0.1164 0.059 Uiso 1 1 calc R . . C15 C 0.8219(5) 1.2945(5) 0.0418(3) 0.0816(18) Uani 1 1 d . . . H15A H 0.8287 1.2556 -0.0013 0.122 Uiso 1 1 calc R . . H15B H 0.8806 1.2755 0.0757 0.122 Uiso 1 1 calc R . . H15C H 0.8310 1.3624 0.0298 0.122 Uiso 1 1 calc R . . C16 C 0.6084(5) 1.3017(4) 0.0230(3) 0.0728(15) Uani 1 1 d . . . H16A H 0.6178 1.3673 0.0053 0.109 Uiso 1 1 calc R . . H16B H 0.5352 1.2961 0.0471 0.109 Uiso 1 1 calc R . . H16C H 0.6111 1.2566 -0.0168 0.109 Uiso 1 1 calc R . . C17 C 0.5518(4) 1.1315(4) 0.1414(3) 0.0563(13) Uani 1 1 d . . . H17 H 0.4998 1.1462 0.1009 0.068 Uiso 1 1 calc R . . C18 C 0.5202(5) 1.1990(5) 0.2037(3) 0.0770(17) Uani 1 1 d . . . H18A H 0.4407 1.1893 0.2165 0.115 Uiso 1 1 calc R . . H18B H 0.5318 1.2659 0.1893 0.115 Uiso 1 1 calc R . . H18C H 0.5683 1.1846 0.2447 0.115 Uiso 1 1 calc R . . C19 C 0.5373(6) 1.0227(5) 0.1607(4) 0.094(2) Uani 1 1 d . . . H19A H 0.5878 1.0064 0.2002 0.141 Uiso 1 1 calc R . . H19B H 0.5565 0.9832 0.1194 0.141 Uiso 1 1 calc R . . H19C H 0.4587 1.0104 0.1745 0.141 Uiso 1 1 calc R . . C20 C 1.1300(4) 1.0547(4) 0.2332(3) 0.0527(12) Uani 1 1 d . . . H20 H 1.1274 1.1030 0.2724 0.063 Uiso 1 1 calc R . . C21 C 1.1593(5) 1.1086(4) 0.1640(3) 0.0769(16) Uani 1 1 d . . . H21A H 1.2317 1.1419 0.1697 0.115 Uiso 1 1 calc R . . H21B H 1.0997 1.1554 0.1535 0.115 Uiso 1 1 calc R . . H21C H 1.1649 1.0625 0.1248 0.115 Uiso 1 1 calc R . . C22 C 1.2226(5) 0.9800(5) 0.2522(4) 0.0804(18) Uani 1 1 d . . . H22A H 1.2240 0.9295 0.2160 0.121 Uiso 1 1 calc R . . H22B H 1.2058 0.9516 0.2985 0.121 Uiso 1 1 calc R . . H22C H 1.2966 1.0118 0.2539 0.121 Uiso 1 1 calc R . . C23 C 0.9613(4) 0.9283(3) 0.3061(2) 0.0528(11) Uani 1 1 d . . . H23 H 1.0167 0.8740 0.3070 0.063 Uiso 1 1 calc R . . C24 C 0.8396(5) 0.8859(4) 0.3034(3) 0.0784(16) Uani 1 1 d . . . H24A H 0.8267 0.8459 0.3454 0.118 Uiso 1 1 calc R . . H24B H 0.8310 0.8469 0.2605 0.118 Uiso 1 1 calc R . . H24C H 0.7844 0.9384 0.3026 0.118 Uiso 1 1 calc R . . C25 C 0.9792(5) 0.9904(4) 0.3737(2) 0.0659(15) Uani 1 1 d . . . H25A H 0.9328 1.0486 0.3705 0.099 Uiso 1 1 calc R . . H25B H 1.0592 1.0084 0.3775 0.099 Uiso 1 1 calc R . . H25C H 0.9570 0.9536 0.4157 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0486(4) 0.0452(4) 0.0406(4) -0.0028(3) 0.0044(3) 0.0090(3) Pt 0.03910(8) 0.04000(8) 0.03217(7) -0.00552(7) -0.00480(7) 0.00483(7) Cl 0.0735(8) 0.0593(7) 0.0492(6) -0.0226(5) -0.0056(6) 0.0057(7) P1 0.0352(6) 0.0420(6) 0.0383(5) -0.0050(5) -0.0031(4) 0.0055(5) P2 0.0448(6) 0.0461(6) 0.0313(5) -0.0035(5) -0.0078(5) 0.0063(5) O1 0.0421(15) 0.0534(17) 0.0373(14) -0.0093(14) -0.0107(12) 0.0112(14) O2 0.0529(17) 0.0464(17) 0.0355(14) -0.0048(12) -0.0132(12) 0.0148(15) O3 0.106(3) 0.072(3) 0.079(3) 0.026(2) 0.008(3) 0.009(3) O4 0.104(4) 0.114(4) 0.095(3) -0.017(3) 0.048(3) 0.028(3) O5 0.066(3) 0.083(3) 0.133(4) -0.010(3) -0.017(3) -0.007(2) C1 0.038(2) 0.041(2) 0.0303(19) -0.0001(16) -0.0037(16) 0.0030(17) C2 0.040(2) 0.038(2) 0.0331(19) -0.0061(16) -0.0018(18) 0.007(2) C3 0.035(2) 0.043(2) 0.035(2) -0.0027(18) -0.0007(17) 0.0072(18) C4 0.033(2) 0.054(2) 0.035(2) -0.0051(19) -0.0072(17) 0.002(2) C5 0.056(3) 0.048(3) 0.042(2) -0.008(2) -0.0040(19) -0.004(2) C6 0.074(3) 0.045(3) 0.048(3) -0.013(2) 0.002(2) 0.000(3) C7 0.072(3) 0.039(2) 0.054(3) 0.000(2) 0.007(2) 0.011(2) C8 0.058(3) 0.043(2) 0.041(2) 0.0008(19) 0.000(2) 0.010(2) C9 0.044(2) 0.038(2) 0.038(2) 0.0044(18) 0.0008(18) 0.0004(19) C10 0.039(2) 0.040(2) 0.039(2) -0.0066(17) 0.0011(17) -0.0018(18) C11 0.066(3) 0.061(3) 0.048(3) 0.002(2) 0.006(2) 0.004(3) C12 0.067(3) 0.073(3) 0.059(3) -0.005(3) 0.008(3) 0.017(3) C13 0.051(3) 0.056(3) 0.073(3) -0.005(3) 0.000(2) 0.006(3) C14 0.053(3) 0.047(3) 0.048(3) 0.000(2) -0.005(2) 0.006(2) C15 0.066(4) 0.081(4) 0.098(4) 0.025(4) 0.012(3) -0.008(3) C16 0.072(4) 0.064(3) 0.082(4) 0.011(3) -0.019(3) 0.010(3) C17 0.036(3) 0.069(3) 0.064(3) -0.011(3) 0.003(2) -0.001(2) C18 0.058(3) 0.098(4) 0.075(4) -0.021(3) 0.026(3) 0.004(3) C19 0.079(4) 0.080(4) 0.124(6) -0.008(4) 0.041(4) -0.027(4) C20 0.053(3) 0.057(3) 0.048(3) -0.005(2) -0.012(2) -0.003(2) C21 0.071(3) 0.073(4) 0.086(4) 0.013(3) 0.003(3) -0.012(4) C22 0.044(3) 0.104(5) 0.093(4) 0.013(4) -0.003(3) 0.009(3) C23 0.060(3) 0.055(3) 0.043(2) 0.004(2) -0.002(2) 0.010(2) C24 0.089(4) 0.072(3) 0.074(4) 0.018(3) 0.002(3) -0.023(4) C25 0.071(3) 0.092(4) 0.035(2) -0.003(3) 0.001(2) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C12 1.825(5) . ? Cr C11 1.831(5) . ? Cr C13 1.832(6) . ? Cr C6 2.202(5) . ? Cr C8 2.206(4) . ? Cr C7 2.206(5) . ? Cr C5 2.233(5) . ? Cr C9 2.294(4) . ? Cr C10 2.330(4) . ? Pt C2 1.967(3) . ? Pt P1 2.2572(11) . ? Pt P2 2.2652(11) . ? Pt Cl 2.3618(10) . ? P1 O1 1.652(3) . ? P1 C17 1.814(5) . ? P1 C14 1.827(5) . ? P2 O2 1.651(3) . ? P2 C20 1.817(5) . ? P2 C23 1.817(4) . ? O1 C3 1.382(5) . ? O2 C1 1.383(4) . ? O3 C11 1.153(6) . ? O4 C12 1.152(6) . ? O5 C13 1.148(6) . ? C1 C2 1.375(5) . ? C1 C9 1.415(6) . ? C2 C3 1.422(6) . ? C3 C4 1.367(6) . ? C4 C10 1.412(6) . ? C5 C6 1.381(7) . ? C5 C10 1.431(6) . ? C6 C7 1.410(7) . ? C7 C8 1.387(6) . ? C8 C9 1.418(6) . ? C9 C10 1.435(6) . ? C14 C16 1.501(7) . ? C14 C15 1.517(7) . ? C17 C18 1.519(7) . ? C17 C19 1.537(8) . ? C20 C21 1.513(7) . ? C20 C22 1.520(7) . ? C23 C25 1.523(6) . ? C23 C24 1.524(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Cr C11 90.0(2) . . ? C12 Cr C13 86.6(2) . . ? C11 Cr C13 90.3(2) . . ? C12 Cr C6 89.8(2) . . ? C11 Cr C6 119.0(2) . . ? C13 Cr C6 150.5(2) . . ? C12 Cr C8 121.9(2) . . ? C11 Cr C8 148.17(19) . . ? C13 Cr C8 90.7(2) . . ? C6 Cr C8 66.60(17) . . ? C12 Cr C7 93.6(2) . . ? C11 Cr C7 155.9(2) . . ? C13 Cr C7 113.7(2) . . ? C6 Cr C7 37.32(17) . . ? C8 Cr C7 36.65(16) . . ? C12 Cr C5 113.3(2) . . ? C11 Cr C5 90.5(2) . . ? C13 Cr C5 160.03(19) . . ? C6 Cr C5 36.28(17) . . ? C8 Cr C5 78.23(17) . . ? C7 Cr C5 66.17(18) . . ? C12 Cr C9 158.2(2) . . ? C11 Cr C9 111.63(19) . . ? C13 Cr C9 95.54(19) . . ? C6 Cr C9 77.69(16) . . ? C8 Cr C9 36.67(15) . . ? C7 Cr C9 65.71(16) . . ? C5 Cr C9 65.70(15) . . ? C12 Cr C10 149.6(2) . . ? C11 Cr C10 87.6(2) . . ? C13 Cr C10 123.66(18) . . ? C6 Cr C10 65.36(16) . . ? C8 Cr C10 65.68(16) . . ? C7 Cr C10 77.39(17) . . ? C5 Cr C10 36.48(14) . . ? C9 Cr C10 36.14(14) . . ? C2 Pt P1 80.99(12) . . ? C2 Pt P2 80.80(12) . . ? P1 Pt P2 161.68(4) . . ? C2 Pt Cl 178.23(13) . . ? P1 Pt Cl 99.37(4) . . ? P2 Pt Cl 98.90(4) . . ? O1 P1 C17 102.6(2) . . ? O1 P1 C14 102.07(18) . . ? C17 P1 C14 107.3(2) . . ? O1 P1 Pt 104.29(11) . . ? C17 P1 Pt 117.10(18) . . ? C14 P1 Pt 120.66(16) . . ? O2 P2 C20 103.5(2) . . ? O2 P2 C23 102.44(18) . . ? C20 P2 C23 107.7(2) . . ? O2 P2 Pt 103.90(10) . . ? C20 P2 Pt 117.97(16) . . ? C23 P2 Pt 118.90(17) . . ? C3 O1 P1 115.8(2) . . ? C1 O2 P2 114.9(2) . . ? C2 C1 O2 118.7(3) . . ? C2 C1 C9 124.2(3) . . ? O2 C1 C9 117.2(3) . . ? C1 C2 C3 116.5(3) . . ? C1 C2 Pt 121.7(3) . . ? C3 C2 Pt 121.8(3) . . ? C4 C3 O1 119.9(4) . . ? C4 C3 C2 123.4(4) . . ? O1 C3 C2 116.7(3) . . ? C3 C4 C10 118.6(4) . . ? C6 C5 C10 121.2(4) . . ? C6 C5 Cr 70.6(3) . . ? C10 C5 Cr 75.5(2) . . ? C5 C6 C7 120.5(4) . . ? C5 C6 Cr 73.1(3) . . ? C7 C6 Cr 71.5(3) . . ? C8 C7 C6 119.8(4) . . ? C8 C7 Cr 71.6(3) . . ? C6 C7 Cr 71.2(3) . . ? C7 C8 C9 121.1(4) . . ? C7 C8 Cr 71.7(3) . . ? C9 C8 Cr 75.1(2) . . ? C1 C9 C8 124.5(4) . . ? C1 C9 C10 116.2(4) . . ? C8 C9 C10 119.3(4) . . ? C1 C9 Cr 130.9(3) . . ? C8 C9 Cr 68.3(2) . . ? C10 C9 Cr 73.3(2) . . ? C4 C10 C5 121.0(4) . . ? C4 C10 C9 121.1(4) . . ? C5 C10 C9 117.9(4) . . ? C4 C10 Cr 131.9(3) . . ? C5 C10 Cr 68.1(2) . . ? C9 C10 Cr 70.6(2) . . ? O3 C11 Cr 178.4(5) . . ? O4 C12 Cr 178.2(6) . . ? O5 C13 Cr 178.6(5) . . ? C16 C14 C15 111.7(4) . . ? C16 C14 P1 114.0(4) . . ? C15 C14 P1 108.2(4) . . ? C18 C17 C19 112.6(5) . . ? C18 C17 P1 110.9(4) . . ? C19 C17 P1 109.6(4) . . ? C21 C20 C22 111.3(5) . . ? C21 C20 P2 109.4(3) . . ? C22 C20 P2 112.9(4) . . ? C25 C23 C24 111.4(4) . . ? C25 C23 P2 110.3(3) . . ? C24 C23 P2 109.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.940 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.081 #==============================================================================